Benzoic Acid → HCID 56984157, 화합물

HRID 1395214노트

반응식

HRID 1395214 반응식
[C:1]([CH:6]1[CH2:11][CH2:10][CH:9]([CH:12]=O)[CH2:8][CH2:7]1)([CH2:4][CH3:5])([CH3:3])[CH3:2].[C:14]([C:19](=P(C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1)[CH3:20])([O:16][CH2:17][CH3:18])=[O:15].C(O)(=O)C1C=CC=CC=1>C1(C)C=CC=CC=1>[CH2:17]([O:16][C:14](=[O:15])[C:19]([CH3:20])=[CH:12][CH:9]1[CH2:8][CH2:7][CH:6]([C:1]([CH2:4][CH3:5])([CH3:2])[CH3:3])[CH2:11][CH2:10]1)[CH3:18]

참가 물질

5

반응물 3

HCID 243Benzoic AcidHCID 79792Ethyl 2-(triphenylphosphoranylidene)propionateHCID 203406004-Tert.amyl-cyclohexane-1-carboxaldehyde

생성물 1

HCID 56984157HCID 56984157, 화합물

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

A mixture of 46.3 g of 4-tert.amyl-cyclohexane-1-carboxaldehyde, 92.3 g of (α-carbethoxy-ethylidene)-triphenyl-phosphorane and 7.6 g of benzoic acid in 250 ml of toluene is heated at reflux for 3.5 hours under nirogen gasification and the toluene is evaporated. The oily-crystalline residue is dissolved in 1600 ml of methanol/water (4:1) and exhaustively extracted with hexane. The combined hexane extracts are washed with sodium carbonate solution and water, dried over sodium sulphate and evaporated. By distillation there is obtained pure 3-(4-tert.amyl-cyclohexyl)-2-methyl-acrylic acid ethyl ester of boiling point 113°-115° C./0.03 Torr.

후처리

  1. temperatureis heated
  2. temperatureat reflux for 3.5 hours under nirogen gasification
  3. customthe toluene is evaporated
  4. dissolutionThe oily-crystalline residue is dissolved in 1600 ml of methanol/water (4:1)
  5. extractionexhaustively extracted with hexane
  6. washThe combined hexane extracts are washed with sodium carbonate solution and water
  7. dry with materialdried over sodium sulphate
  8. customevaporated
  9. distillationBy distillation there

출처 및 근거

ORD 기록
ord-b5aefe35b1e94d719a364b9f83476dfd
출처 데이터셋
uspto-grants-1980_05
특허 번호
US04202894

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