(Bis(2-methoxyethyl)amino)sulfur trifluoride → HCID 53419027, 화합물

HRID 245139

반응식

HRID 245139 반응식
COCCN(S(F)(F)[F:11])CCOC.O[CH:15]1[CH2:20][CH2:19][N:18]([CH:21]2[CH2:26][CH2:25][N:24]([C:27]([O:29][C:30]([CH3:33])([CH3:32])[CH3:31])=[O:28])[CH2:23][CH2:22]2)[CH2:17][CH2:16]1>>[F:11][CH:15]1[CH2:20][CH2:19][N:18]([CH:21]2[CH2:26][CH2:25][N:24]([C:27]([O:29][C:30]([CH3:33])([CH3:32])[CH3:31])=[O:28])[CH2:23][CH2:22]2)[CH2:17][CH2:16]1

참가 물질

3

반응물 2

HCID 2734690(Bis(2-methoxyethyl)amino)sulfur trifluorideHCID 9835508tert-Butyl 4-hydroxy-[1,4'-bipiperidine]-1'-carboxylate

생성물 1

HCID 53419027HCID 53419027, 화합물수율 60%

반응 조건

온도
-78 °C

실험 절차

Deoxo-Fluor® was added to a solution of 1,1-dimethylethyl 4-hydroxy-1,4′-bipiperidine-1′-carboxylate (0.500 g, 1.76 mmol) dropwise at −78° C. The mixture was maintained at −78° C. for 30 min before it was warmed to room temperature and stirred for 2 h. The mixture was washed with saturated aqueous sodium bicarbonate. The organic phase was dried over Na2SO4, filtered, and concentrated in vacuo. The crude material was purified via column chromatography (1:200 methanol/methylene chloride) to afford 1,1-dimethylethyl 4-fluoro-1,4′-bipiperidine-1′-carboxylate (0.300 g, 60% yield) as a colorless oil.

후처리

  1. temperaturewas warmed to room temperature
  2. washThe mixture was washed with saturated aqueous sodium bicarbonate
  3. dry with materialThe organic phase was dried over Na2SO4
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo
  6. customThe crude material was purified via column chromatography (1:200 methanol/methylene chloride)

출처 및 근거

ORD 기록
ord-75d10dc72c0c4ec2945bb9e80a22e50c
출처 데이터셋
uspto-grants-2014_02
특허 번호
US08658636B2

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