홈MCP워크벤치Skills
홈워크벤치알림마이페이지
llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
  1. 홈
  2. /반응

Potassium Hydroxide → Ethyl 2-benzylacrylate

HRID 36373
노트
인쇄 미리보기

반응식

HRID 36373 반응식
[OH-].[K+].[CH2:3]([O:5][C:6](=[O:20])[CH:7]([CH2:13][C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)[C:8](OCC)=O)[CH3:4]>C(O)C>[CH2:8]=[C:7]([CH2:13][C:14]1[CH:15]=[CH:16][CH:17]=[CH:18][CH:19]=1)[C:6]([O:5][CH2:3][CH3:4])=[O:20]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 14797Potassium HydroxideHCID 69090Diethyl 2-benzylpropanedioate

생성물 1

HCID 11084648Ethyl 2-benzylacrylate수율 85.5%

시약·촉매·용매 1

HCID 702Ethanol용매2회

실험 절차

A mixture of of KOH (8.5 g) in ethanol (100 mL) was added at room temperature to benzylmalonic acid diethyl ester (40 g) in ethanol (80 mL) and the solution was stirred at room temperature overnight, then concentrated by evaporation. Water (14 mL) was added and then the mixture was acidified in an ice bath with concentrated hydrochloric acid (12.6 mL). The mixture was partitioned between water and ether; the organic phase was separated, dried and the ether was evaporated. The residue was treated with pyridine (26 mL), piperidine (1.22 g) and paraformaldehyde (3.56 g). The mixture was heated in an oil bath (130°) for 90 minutes, then cooled, and water (440 mL) was added. The mixture was extracted 3 times with n-hexane (150 mL). The combined organic phases were washed successively with water, 1N HCl, water, saturated NaHCO3 solution and brine. The organic solution was dried (MgSO4) and evaporated to give the title compound as colorless oil (26 g, 85 % yield). 1H NMR: 300MHz spectrum consistent with proposed structure.

후처리

  1. concentrationconcentrated by evaporation
  2. additionWater (14 mL) was added
  3. customthe mixture was acidified in an ice bath with concentrated hydrochloric acid (12.6 mL)
  4. customThe mixture was partitioned between water and ether
  5. customthe organic phase was separated
  6. customdried
  7. customthe ether was evaporated
  8. additionThe residue was treated with pyridine (26 mL), piperidine (1.22 g) and paraformaldehyde (3.56 g)
  9. temperatureThe mixture was heated in an oil bath (130°) for 90 minutes
  10. temperaturecooled
  11. additionwater (440 mL) was added
  12. extractionThe mixture was extracted 3 times with n-hexane (150 mL)
  13. washThe combined organic phases were washed successively with water, 1N HCl, water, saturated NaHCO3 solution and brine
  14. dry with materialThe organic solution was dried (MgSO4)
  15. customevaporated

출처 및 근거

ORD 기록
ord-0924ded253b34cb1b6e3517fb0eb3cab
출처 데이터셋
uspto-grants-1995_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05414018

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트