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

1,3-Butadiene → Cyclopropanecarboxylic acid, 2-ethenyl-, ethyl ester

HRID 704638
노트
인쇄 미리보기

반응식

HRID 704638 반응식
[N+](=[CH:3][C:4]([O:6][CH2:7][CH3:8])=[O:5])=[N-].[CH2:9]=[CH:10][CH:11]=[CH2:12]>CC(O)=O.CC(O)=O.CC(O)=O.CC(O)=O.[Rh].[Rh]>[CH:10]([CH:11]1[CH2:12][CH:3]1[C:4]([O:6][CH2:7][CH3:8])=[O:5])=[CH2:9]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 78451,3-ButadieneHCID 12192Ethyl diazoacetate

생성물 1

HCID 12261391Cyclopropanecarboxylic acid, 2-ethenyl-, ethyl ester수율 76%

시약·촉매·용매 1

HCID 423677Acetic acid, rhodium salt (4:2)촉매

실험 절차

Butadiene (200 mL) was liquified at -70° C. and added to ethyl diazoacetate (20 g, 175 mmol) in a pressure vessel. The catalyst, rhodium (II) acetate dimer (300 mg, 0.7 mmol), was added and the reaction vessel sealed. The reaction mixture was allowed to warm to ambient temperature and the reaction vessel was shaken for 24 h at ambient temperature. The reaction mixture and the ethanol rinse of the reaction vessel were combined and this blue solution was filtered through 50 g of silica gel. The silica gel was washed with 2% diethyl ether in pentane until the blue color was eluted. The blue solution was then concentrated in vacuo at 0° C. and filtered through CeliteR filter aid to remove any remaining catalyst. The filtrate was distilled under reduced pressure (approximately 15 mm) to yield 18.6 g (76% yield) of ethyl 2-ethenylcyclopropane carboxylate as a clear colorless liquid, b.p. 22°-26° C.

후처리

  1. customwas liquified at -70° C.
  2. customthe reaction vessel sealed
  3. washThe reaction mixture and the ethanol rinse of the reaction vessel
  4. filtrationthis blue solution was filtered through 50 g of silica gel
  5. washThe silica gel was washed with 2% diethyl ether in pentane until the blue color
  6. washwas eluted
  7. concentrationThe blue solution was then concentrated in vacuo at 0° C.
  8. filtrationfiltered through CeliteR
  9. filtrationfilter aid
  10. customto remove any remaining catalyst
  11. distillationThe filtrate was distilled under reduced pressure (approximately 15 mm)

출처 및 근거

ORD 기록
ord-d750da86e4ec45f2b0a29c2889d003bf
출처 데이터셋
uspto-grants-1991_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04988703

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트