Potassium Hydroxide → HCID 53942620、化合物

HRID 971876ノート

反応式

HRID 971876 の反応式
[CH3:1][CH2:2][O:3][C:4]([CH:6]1[C:10](=[O:11])[CH2:9][CH2:8][CH2:7]1)=[O:5].Cl[CH2:13][C:14]1[CH:19]=[CH:18][C:17]([CH2:20][C:21]([O:23][CH2:24][CH3:25])=[O:22])=[CH:16][CH:15]=1.[OH-].[K+]>CN(C)C=O.C(O)(=O)C>[CH2:2]([O:3][C:4]([C:6]1([CH2:13][C:14]2[CH:15]=[CH:16][C:17]([CH2:20][C:21]([O:23][CH2:24][CH3:25])=[O:22])=[CH:18][CH:19]=2)[CH2:7][CH2:8][CH2:9][C:10]1=[O:11])=[O:5])[CH3:1]

参加物

6

反応物 3

HCID 14797Potassium HydroxideHCID 69136Ethyl 2-oxocyclopentanecarboxylateHCID 12799528Ethyl [4-(chloromethyl)phenyl]acetate

生成物 1

HCID 53942620HCID 53942620、化合物収率 72.4%

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒HCID 6228Dimethylformamide溶媒2 回

反応条件

温度
50 °C

実験手順

A mixture of 9.4 g of ethyl 2-cyclopentanonecarboxylate, 10.6 g of ethyl p-chloromethylphenylacetate, 3.58 g of potassium hydroxide and 60 ml of dimethyl formamide was stirred at room temperature for 5 hours, at 50° C. for 1 hour and thereafter at room temperature overnight. The reaction mixture was acidified by addition of acetic acid, dimethyl formamide was removed by distillation, water was added to the residue, and the mixture was extracted with ether. The extract was washed with water, dried over anhydrous sodium sulfate, and the solvent evaporated to give an oily substance, which was subjected to a vacuum distillation affording 12 g of the desired compound, b.p. 180°-190° C. at 0.8 mm Hg.

後処理

  1. customat room temperature
  2. customovernight
  3. customwas removed by distillation, water
  4. additionwas added to the residue
  5. extractionthe mixture was extracted with ether
  6. washThe extract was washed with water
  7. dry with materialdried over anhydrous sodium sulfate
  8. customthe solvent evaporated
  9. customto give an oily substance, which
  10. distillationwas subjected to a vacuum distillation

出典と根拠

ORDレコード
ord-381acb6715ca46f4bf5cfc5408467c13
出典データセット
uspto-grants-1979_07
特許番号
US04161538

反応ノート

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