Benzoic Acid → HCID 56984157、化合物

HRID 1395214ノート

反応式

HRID 1395214 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

HCID 56984157HCID 56984157、化合物

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-b5aefe35b1e94d719a364b9f83476dfd
出典データセット
uspto-grants-1980_05
特許番号
US04202894

反応ノート

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