Water → Isopropenyl hydrogen sebacate

HRID 443996

반응식

HRID 443996 반응식
CN1C[CH2:5][CH2:4][C:3]1=O.[C:8]([OH:21])(=[O:20])[CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][C:17]([OH:19])=[O:18].O.[Cl-].[NH4+].CC#C.C=C=C>C/C(/[O-])=C/C(C)=O.C/C(/[O-])=C/C(C)=O.[Zn+2]>[C:8]([O:21][C:4]([CH3:5])=[CH2:3])(=[O:20])[CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][C:17]([OH:19])=[O:18]

참가 물질

7

반응물 5

HCID 962WaterHCID 5192Sebacic AcidHCID 13387N-methyl-2-pyrrolidoneHCID 25517Ammonium ChlorideHCID 62152Propyne, mixed with propadiene

생성물 1

HCID 23466329Isopropenyl hydrogen sebacate

시약·촉매·용매 1

HCID 5360437zinc;(Z)-4-oxopent-2-en-2-olate촉매

실험 절차

A 1-liter pressure vessel equipped with a magnetic stirrer, a thermocouple, a thermocontroller, a methyl acetylene reservoir tank, a pressure burette, a gas line, and a control valve, was flushed free of air with nitrogen and charged with 100 ml (1.04 moles) of N-methyl-2-pyrrolidone; 10.0 gm (0.0038 moles) of zinc acetylacetonate; 25.0 gm. (0.12 moles) sebacic acid; 11.0 gms (0.61 moles) water; 5.0 gm (0.093 moles) ammonium chloride; and 135 ml of MAPP gas (65 mole percent methyl acetylene and allene), and heated to 155° C. at a maximum pressure of 550 psi with stirring for about 14 hours. The reaction vessel was allowed to cool at room temperature and an aliquot removed. The aliquot was shaken with diethyl ether and water and the ether layer dried with magnesium sulphate and evaporated to dryness. An infrared spectrum of the dried product in carbon disulphide solution showed quantitative conversion to isopropenyl hydrogen sebacate. The IR spectrum was identical to that of a pure reference sample.

후처리

  1. customA 1-liter pressure vessel equipped with a magnetic stirrer
  2. customa thermocouple, a thermocontroller, a methyl acetylene reservoir tank, a pressure burette, a gas line, and a control valve, was flushed free of air with nitrogen
  3. customan aliquot removed
  4. stirringThe aliquot was shaken with diethyl ether and water
  5. dry with materialthe ether layer dried with magnesium sulphate
  6. customevaporated to dryness

출처 및 근거

ORD 기록
ord-dba9dced6cf14cf09533deab79e11c3e
출처 데이터셋
uspto-grants-1981_04
특허 번호
US04262137

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