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

Methanol → N[2-(Bromoacetyl-phenyl)-1,1-dimethyl-ethyl]-2,2,2-trifluoroacetamide

HRID 49385
노트
인쇄 미리보기

반응식

HRID 49385 반응식
[CH3:1][C:2]([NH:11][C:12](=[O:17])[C:13]([F:16])([F:15])[F:14])([CH3:10])[CH2:3][C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1.[Br-:18].[Br-].[Br-].C([N+](CC[CH2:36][CH3:37])(CCCC)CCCC)CCC.C([N+](CCCC)(CCCC)CCCC)CCC.C([N+](CCCC)(CCCC)CCCC)CCC.C[OH:73]>C(Cl)Cl>[Br:18][CH2:36][C:37]([C:5]1[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=1[CH2:3][C:2]([NH:11][C:12](=[O:17])[C:13]([F:16])([F:14])[F:15])([CH3:1])[CH3:10])=[O:73]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 887MethanolHCID 592937N-(1,1-Dimethyl-2-phenylethyl)-2,2,2-trifluoroacetamideHCID 23500184Tetra-n-butylammonium tribromide

생성물 1

HCID 18523616N[2-(Bromoacetyl-phenyl)-1,1-dimethyl-ethyl]-2,2,2-trifluoroacetamide수율 41%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

In a round-bottomed flask, N-(1,1-dimethyl-2-phenyl-ethyl)-2,2,2-trifluoroacetamide (6.90 g, 21.0 mmol) was dissolved in methylene chloride (66 ml) and methanol (33 ml). Tetrabutylammonium tribromide (10.6 g, 22.0 mmol) was added to this solution in one portion, and the mixture was allowed to stir at room temperature overnight. The volatiles were then removed in vacuo to an oil, which was then resuspended in 100 ml of methylene chloride and extracted with 125 ml of saturated aqueous sodium bicarbonate. The aqueous extracts were reextracted with methylene chloride (3×10 ml), and the combined organic extracts were then washed with water and dried over magnesium sulfate, filtered, and concentrated in vacuo. The crude oil was purified by column chromatography (silica gel; 60% methylene chloride/hexanes to 10% ethyl acetate/methylene chloride), and the resulting material (5.18 g) was recrystallized from hexanes to afford 3.14 g (41% yield) of pure product as a fluffy white solid.

후처리

  1. customThe volatiles were then removed in vacuo to an oil, which
  2. extractionextracted with 125 ml of saturated aqueous sodium bicarbonate
  3. washthe combined organic extracts were then washed with water
  4. dry with materialdried over magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo
  7. customThe crude oil was purified by column chromatography (silica gel; 60% methylene chloride/hexanes to 10% ethyl acetate/methylene chloride)
  8. customthe resulting material (5.18 g) was recrystallized from hexanes

출처 및 근거

ORD 기록
ord-9b7976b5ab774ad9a591a55bd2fd3c9b
출처 데이터셋
uspto-grants-2004_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06706743B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트