Water → 3-fluoro-N-methyl-N-(trifluoroacetyl)benzylamine

HRID 928031노트

반응식

HRID 928031 반응식
[F:1][C:2]1[CH:3]=[C:4]([CH:13]=[CH:14][CH:15]=1)[CH2:5][NH:6][C:7](=[O:12])[C:8]([F:11])([F:10])[F:9].[H-].[Na+].I[CH3:19].O>C1COCC1>[F:1][C:2]1[CH:3]=[C:4]([CH:13]=[CH:14][CH:15]=1)[CH2:5][N:6]([CH3:19])[C:7](=[O:12])[C:8]([F:10])([F:11])[F:9]

참가 물질

6

반응물 4

HCID 962WaterHCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 624921483-Fluoro-N-trifluoroacetylbenzylamine2회

생성물 1

HCID 627348703-fluoro-N-methyl-N-(trifluoroacetyl)benzylamine수율 92%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

A solution of 3-fluoro-N-(trifluoroacetyl)benzylamine (Intermediate 105, 0.508 g) in THF (5 mL) was added to a stirred suspension of sodium hydride (60% oil dispersion, 0.096 g) in THF (5 mL). The resultant mixture was stirred at room temperature for 30 minutes. Iodomethane (0.653 g) was added and the mixture was stirred at room temperature overnight. The mixture was poured into water and extracted with ethyl acetate, washed with water, dried (MgSO4) and filtered. The filtrate was evaporated to dryness to give 3-fluoro-N-methyl-N-(trifluoroacetyl)benzylamine (0.497 g) as a white solid.

후처리

  1. extractionextracted with ethyl acetate
  2. washwashed with water
  3. dry with materialdried (MgSO4)
  4. filtrationfiltered
  5. customThe filtrate was evaporated to dryness

출처 및 근거

ORD 기록
ord-0bd5bbee307648fbbe32583163ac0e4f
출처 데이터셋
uspto-grants-2016_03
특허 번호
US09290472B2

반응 노트

불러오는 중…