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

Diazomethane → HCID 22235737, 화합물

HRID 1744148
노트
인쇄 미리보기

반응식

HRID 1744148 반응식
[CH3:1][C:2](=[CH2:10])[CH2:3][CH2:4][C:5]([O:7][CH2:8][CH3:9])=[O:6].[N+](=[CH2:13])=[N-]>CCOCC.C([O-])(=O)C.[Pd+2].C([O-])(=O)C>[CH3:10][C:2]1([CH2:3][CH2:4][C:5]([O:7][CH2:8][CH3:9])=[O:6])[CH2:13][CH2:1]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 9550DiazomethaneHCID 3416433Ethyl 4-methyl-4-pentenoate

생성물 1

HCID 22235737HCID 22235737, 화합물

시약·촉매·용매 2

HCID 167845palladium(II) acetate촉매HCID 3283Diethyl Ether용매

실험 절차

To an ice cold solution of ethyl 4-methyl-4-pentenoate (1.11 g, 7.8 mmol) in 0.5 M diazomethane in Et2O, was added palladium(II) acetate by portionwise addition (4 portions of 5 mg each were added in 15 min intervals). A total of 4 portions were added. The reaction mixture was filtered on a pad of celite and concentrated under 60 mm Hg with gentle warming. This crude product was treated a second time with diazomethane and palladium(II) acetate, filtered and concentrated. The resulting oil was filtered on a pad of florisil (60–100 mesh), washed with Et2O (2×10 mL), concentrated under 60 mm Hg to give ethyl 3-(1-methylcyclopropyl)propanoate as a colorless oil.

후처리

  1. additionby portionwise addition (4 portions of 5 mg each were added in 15 min intervals)
  2. additionA total of 4 portions were added
  3. filtrationThe reaction mixture was filtered on a pad of celite
  4. concentrationconcentrated under 60 mm Hg with gentle warming
  5. additionThis crude product was treated a second time with diazomethane and palladium(II) acetate
  6. filtrationfiltered
  7. concentrationconcentrated
  8. filtrationThe resulting oil was filtered on a pad of florisil (60–100 mesh)
  9. washwashed with Et2O (2×10 mL)
  10. concentrationconcentrated under 60 mm Hg

출처 및 근거

ORD 기록
ord-3eed97af006a419ebac1c3da9a8d28d9
출처 데이터셋
uspto-grants-2006_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07012075B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트