Potassium Hydroxide → HCID 53942620, 화합물

HRID 971876노트

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HRID 971876 반응식
[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]

참가 물질

6

반응물 3

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

생성물 1

HCID 53942620HCID 53942620, 화합물수율 72.4%

시약·촉매·용매 2

HCID 176Acetic Acid용매HCID 6228Dimethylformamide용매2회

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온도
50 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-381acb6715ca46f4bf5cfc5408467c13
출처 데이터셋
uspto-grants-1979_07
특허 번호
US04161538

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