3-Methoxybenzylamine → HCID 57754052, 화합물

HRID 226213

반응식

HRID 226213 반응식
[C:1]([O:5][C:6](=[O:21])[NH:7][C@@H:8]([C@H:18]1[CH2:20][O:19]1)[CH2:9][C:10]1[CH:15]=[CH:14][C:13]([F:16])=[C:12]([F:17])[CH:11]=1)([CH3:4])([CH3:3])[CH3:2].[O-]S(C(F)(F)F)(=O)=O.[Li+].[CH3:31][O:32][C:33]1[CH:34]=[C:35]([CH:38]=[CH:39][CH:40]=1)[CH2:36][NH2:37].[Cl-].[NH4+]>C(#N)C>[C:1]([O:5][C:6](=[O:21])[NH:7][C@@H:8]([CH2:9][C:10]1[CH:15]=[CH:14][C:13]([F:16])=[C:12]([F:17])[CH:11]=1)[C@H:18]([OH:19])[CH2:20][NH:37][CH2:36][C:35]1[CH:38]=[CH:39][CH:40]=[C:33]([O:32][CH3:31])[CH:34]=1)([CH3:4])([CH3:3])[CH3:2]

참가 물질

6

반응물 4

HCID 211563-MethoxybenzylamineHCID 25517Ammonium ChlorideHCID 3664839Trifluoromethanesulfonic acid, lithium saltHCID 86616462(1R,2S)-[2-(3,4-difluoro-phenyl)-1-oxiranyl-ethyl]-carbamic acid tert-butyl ester

생성물 1

HCID 57754052HCID 57754052, 화합물

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

A solution of (1R,2S)-[2-(3,4-difluoro-phenyl)-1-oxiranyl-ethyl]-carbamic acid tert-butyl ester (0.03 g, 0.1 mmol) in acetonitrile (1 mL) was treated with lithium triflate (0.032 g, 0.2 mmol) and stirred at ambient temperature for 20 minutes. Then 3-methoxybenzylamine (0.016 mL, 0.12 mmol) was added to the reaction neat in one portion. The reaction was stirred at ambient temperature for 14 hours. The reaction was poured into saturated ammonium chloride solution (5 mL), extracted with ethyl acetate, the organic phase separated, dried (MgSO4) and the solvent removed at reduced pressure. The product was obtained as an oil and used without further purification (0.041 g, 94%). MS: 437 (M+H, 100%).

후처리

  1. stirringThe reaction was stirred at ambient temperature for 14 hours
  2. extractionextracted with ethyl acetate
  3. customthe organic phase separated
  4. dry with materialdried (MgSO4)
  5. customthe solvent removed at reduced pressure
  6. customThe product was obtained as an oil
  7. customused without further purification (0.041 g, 94%)

출처 및 근거

ORD 기록
ord-102b0fd138274c048ebe5de232edecef
출처 데이터셋
uspto-grants-2009_07
특허 번호
US07557137B2

연결된 노트

불러오는 중…