Benzoic Acid → 3-(4-Tert.butyl-cyclohexyl)-2-methyl-acrylic acid ethyl ester

HRID 1733275

반응식

HRID 1733275 반응식
[C:1]([CH:5]1[CH2:10][CH2:9][CH:8]([CH:11]=O)[CH2:7][CH2:6]1)([CH3:4])([CH3:3])[CH3:2].[C:13]([C:18](=P(C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1)[CH3:19])([O:15][CH2:16][CH3:17])=[O:14].C(O)(=O)C1C=CC=CC=1>C1(C)C=CC=CC=1.CO.O>[CH2:16]([O:15][C:13](=[O:14])[C:18]([CH3:19])=[CH:11][CH:8]1[CH2:7][CH2:6][CH:5]([C:1]([CH3:2])([CH3:3])[CH3:4])[CH2:10][CH2:9]1)[CH3:17]

참가 물질

6

반응물 3

HCID 243Benzoic AcidHCID 79792Ethyl 2-(triphenylphosphoranylidene)propionateHCID 88655Cyclohexanecarboxaldehyde, 4-(1,1-dimethylethyl)-

생성물 1

HCID 569892053-(4-Tert.butyl-cyclohexyl)-2-methyl-acrylic acid ethyl ester

시약·촉매·용매 2

HCID 1140Toluene용매2회HCID 22242641Methanol--water (1/1)용매

실험 절차

A mixture of 20.2 g of 4-tert.butyl-cyclohexane-1-carboxaldehyde, 52 g of (α-carbethoxy-ethylidene)-triphenyl-phosphorane and 3.6 g of benzoic acid in 120 ml of toluene is heated at reflux for 16 hours under nitrogen gasification and the toluene is evaported. The oily-crystalline residue is dissolved in 600 ml of methanol/water (4:1) and exhaustively extracted with hexane. The combined hexane extracts are washed with sodium bicarbonate solution and water, dried over sodium sulphate and evaporated. By distillation there is obtained pure 3-(4-tert.butyl-cyclohexyl)-2-methyl-acrylic acid ethyl ester of boiling point 99° C./0.03 Torr.

후처리

  1. temperatureis heated
  2. temperatureat reflux for 16 hours under nitrogen gasification
  3. extractionexhaustively extracted with hexane
  4. washThe combined hexane extracts are washed with sodium bicarbonate solution and water
  5. dry with materialdried over sodium sulphate
  6. customevaporated
  7. distillationBy distillation there

출처 및 근거

ORD 기록
ord-371e8a1fcf7f4418af5fe2f16400894e
출처 데이터셋
uspto-grants-1980_12
특허 번호
US04241058

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