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

Hydrochloric Acid → 5-(1,1-Difluoroethyl)-2-(trifluoromethoxy)benzaldehyde

HRID 1634328
노트
인쇄 미리보기

반응식

HRID 1634328 반응식
[F:1][C:2]([C:5]1[CH:6]=[CH:7][C:8]([O:13][C:14]([F:17])([F:16])[F:15])=[C:9]([CH:12]=1)[C:10]#N)([F:4])[CH3:3].[OH2:18].Cl>C(Cl)Cl>[F:1][C:2]([C:5]1[CH:6]=[CH:7][C:8]([O:13][C:14]([F:17])([F:16])[F:15])=[C:9]([CH:12]=1)[CH:10]=[O:18])([F:4])[CH3:3]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 962WaterHCID 186776385-(1,1-Difluoroethyl)-2-(trifluoromethoxy)benzonitrile

생성물 1

HCID 186776085-(1,1-Difluoroethyl)-2-(trifluoromethoxy)benzaldehyde수율 88%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

반응 조건

온도
0 °C

실험 절차

To a stirred solution of Compound 24 (1.31 g, 5.22 mmol) in dry CH2Cl2(20 ml) was added a solution of diisobutylaluminum hydride(DIBAL) (6.20 ml, 6.26 mmol, 1.01M in toluene solution) with ice-cooling. The reaction mixture was stirred at 0° C. for 3 h. To the mixture was added H2O(6 ml), followed by 6M HCl aq. (20 ml) and stirred at room temperature for 1.5 h. The organic layer was separated and the aqueous layer was extracted with CH2Cl2. The combined solution was washed with sat. NaHCO3 aq. and brine, dried(MgSO4) and concentrated in vacuo to give crude product. The crude product was purified by column chromatography on silica gel with hexane-ethyl acetate (50:1-30:1) to give Compound 25 (1.17 g, 88%) as a yellow oil.

후처리

  1. temperaturecooling
  2. stirringstirred at room temperature for 1.5 h
  3. customThe organic layer was separated
  4. extractionthe aqueous layer was extracted with CH2Cl2
  5. washThe combined solution was washed with sat. NaHCO3 aq. and brine, dried(MgSO4)
  6. concentrationconcentrated in vacuo
  7. customto give crude product
  8. customThe crude product was purified by column chromatography on silica gel with hexane-ethyl acetate (50:1-30:1)

출처 및 근거

ORD 기록
ord-e29c891a480e4fba8bc68dfae4669c79
출처 데이터셋
uspto-grants-2003_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06506775B1

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트