摘要:
1,3-Propanediol is prepared in a process comprising the steps of:contacting, in an essentially non-water-miscible organic solvent, ethylene oxide with carbon monoxide and hydrogen in the presence of a catalytic amount of a non-phosphine-ligated cobalt compound and an effective amount of a lipophilic quaternary phosphonium salt promoter at a temperature within the range of about 50.degree. to about 100.degree. C. and a pressure within the range of about 500 to about 5000 psig, to produce an intermediate product mixture comprising less than 15 wt % 3-hydroxypropanal;adding an aqueous liquid to said intermediate product mixture and extracting into said aqueous liquid a major portion of the 3-hydroxypropanal at a temperature less than about 100.degree. C. to provide an aqueous phase comprising 3-hydroxypropanal in greater concentration than the concentration of 3-hydroxypropanal in the intermediate product mixture, and an organic phase comprising at least a portion of the cobalt compound and at least a portion of the lipophilic quaternary phosphonium salt;contacting the aqueous phase comprising 3-hydroxypropanal with hydrogen in the presence of a hydrogenation catalyst at a pressure of at least about 100 psig and a temperature during at least a portion of the hydrogenation step of at least 40.degree. C. to provide a hydrogenation product mixture comprising 1,3-propanediol.
摘要:
1,3-propanediol is prepared in a process comprising the steps of:contacting ethylene oxide with carbon monoxide and hydrogen in an essentially non-water-miscible solvent in the presence of an effective amount of a non-phosphine-ligated cobalt catalyst and an effective amount of a lipophilic phenol at a temperature within the range of about 50.degree. to about 100.degree. C. and a pressure within the range of about 500 to about 5000 psig, under reaction conditions effective to produce an intermediate product mixture comprising less than about 15 wt % 3-hydroxypropanal;adding an aqueous liquid to said intermediate product mixture and extracting into said aqueous liquid at a temperature less than about 100.degree. C. a major portion of the 3-hydroxypropanal so as to provide an aqueous phase comprising 3-hydroxypropanal in greater concentration than the concentration of 3-hydroxypropanal in said intermediate product mixture and an organic phase comprising at least a portion of the cobalt catalyst or a cobalt-containing derivative thereof and at least a portion of the lipophilic phenol;contacting the aqueous phase comprising 3-hydroxypropanal with hydrogen in the presence of a hydrogenation catalyst at a pressure of at least about 100 psig and a temperature during at least a portion of the hydrogenation step of at least 40.degree. C. to provide a hydrogenation product mixture comprising 1,3-propanediol.
摘要:
1,3-propanediol is prepared in a process comprising the steps of:contacting ethylene oxide with carbon monoxide and hydrogen in an essentially non-water-miscible solvent in the presence of an effective amount of a non-phosphine-ligated cobalt catalyst and an effective amount of a lipophilic quaternary ammonium salt at a temperature within the range of about 50.degree. to about 100.degree. C. and a, pressure within the range of about 500 to about 5000 psig, under reaction conditions effective to produce an intermediate product mixture comprising less than 15 wt % 3-hydroxypropanal;adding an aqueous liquid to said intermediate product mixture and extracting into said aqueous liquid at a temperature less than about 100.degree. C. a major portion of the 3-hydroxypropanal so as to provide an aqueous phase comprising 3-hydroxypropanal in greater concentration than the-concentration of 3-hydroxypropanal in said intermediate product mixture and an organic phase comprising at least a portion of the cobalt catalyst or a cobalt-containing derivative thereof and at least a portion of the lipophilic quaternary ammonium salt;contacting the aqueous phase comprising 3-hydroxypropanal with hydrogen in, the presence of a hydrogenation catalyst at a pressure of at least about 100 psig and a temperature during at least a portion of the hydrogenation step of at least 40.degree. C. to provide a hydrogenation product mixture comprising 1,3-propanediol.
摘要:
The reaction of dimethylformamide, R.sup.1 R.sup.2 R.sup.3 SiX and RY in the presence of zinc or the reaction of dimethylformamide, R.sup.1 R.sup.2 R.sup.3 SiX and a zinc compound RZnY.yL affords hemiaminals of formula I ##STR1## R is e.g. polyhalogenated alkyl containing at least one fluorine atom; R.sup.1, R.sup.2 and R.sup.3 are e.g. alkyl; L is a ligand; X is chlorine or bromine; Y is chlorine, bromine or iodine and y is 1 or 2.
摘要:
A liquid crystal compound of Formula (1) is provided. In Formula (1), R is hydrogen, linear or branching C1-15 alkyl, linear or branching C1-15 alkyl (wherein any one of —CH2— is replaced by —O—, —S—, —CO—, —CO—O—, or —O—CO—), linear or branching C2-15 alkenyl, or linear or branching C2-15 alkenyl (wherein any one of —CH2— is replaced by —O—, —S—, —CO—, —CO—O—, or —O—CO—), A and B are, independently, cyclohexane, cyclohexane (wherein any one of —CH2— is replaced by —O— or —NH—), benzene, or benzene (wherein any one of —CH2═ is replaced by —N═), X is a single bond, —CO—O—, —O—CO—, —CH2O—, —OCH2—, —CH2CH2—, —C═C—, —C≡C—, —CF2O—, or —OCF2—, Q is oxygen or CH2, Y is CF3, CF2H, or CFH2, L1, L2, and L3 are, independently, hydrogen or fluorine, and m is 0, 1, or 2.
摘要:
1,3-propanediol is prepared in a process comprising the steps of:(a) contacting ethylene oxide with carbon monoxide and hydrogen in an essentially non-water-miscible solvent in the presence of an effective amount of a non-phosphine-ligated cobalt catalyst and an effective amount of a lipophilic arsine at a temperature within the range of about 50 to about 100.degree. C. and a pressure within the range of about 500 to about 5000 psig, under reaction conditions effective to produce an intermediate product mixture comprising less than about 15 wt % 3-hydroxypropanal;(b) adding an aqueous liquid to said intermediate product mixture and extracting into said aqueous liquid at a temperature less than about 100.degree. C. a major portion of the 3-hydroxypropanal so as to provide an aqueous phase comprising 3-hydroxypropanal in greater concentration than the concentration of 3-hydroxypropanal in said intermediate product mixture and an organic phase comprising at least a portion of the cobalt catalyst or a cobalt-containing derivative thereof and at least a portion of the lipophilic arsine;(c) separating the aqueous phase from the organic phase;(d) contacting the aqueous phase comprising 3-hydroxypropanal with hydrogen in the presence of a hydrogenation catalyst at a pressure of at least about 100 psig and a temperature during at least a portion of the hydrogenation step of at least 40.degree. C. to provide a hydrogenation product mixture comprising 1,3-propanediol;(e) recovering 1,3-propanediol from said hydrogenation product mixture; and(f) returning at least a portion of the organic phase comprising cobalt compound and lipophilic arsine to the process of step (a).The process enables the production of 1,3-propanediol in high yields and selectivity without the use of a phosphine-ligated cobalt catalyst.
摘要:
A 5-bromo-1-pentanal compound of the formula (I): ##STR1## wherein R.sup.1 and R.sup.2 respectively represent, independently from each other, a member selected from the group consisting of a hydrogen atom and alkyl radicals having 1 to 7 carbon atoms, or an acetal derivative of said 5-bromo-1-pentanal compound, is produced by subjecting a starting compound selected from the group consisting of 4-pentenal compounds of the formula (II): ##STR2## wherein R.sup.1 and R.sup.2 are as defined above, and acetal derivatives of the above-mentioned compounds, to a free radical addition reaction with hydrogen bromide in a liquid medium at a temperature of 10.degree. C. to 60.degree. C.; in the presence of a free radical initiator or by irradiating ultraviolet rays to the reaction mixture, and by collecting the resultant reaction product from the reaction mixture.