Triethylamine → Methanesulfonic acid 1-(2-isopropoxy-5-methanesulfonyl-benzoyl)-piperidin-4-yl ester

HRID 1711734노트

반응식

HRID 1711734 반응식
[OH:1][CH:2]1[CH2:7][CH2:6][N:5]([C:8]([C:10]2[CH:15]=[C:14]([S:16]([CH3:19])(=[O:18])=[O:17])[CH:13]=[CH:12][C:11]=2[O:20][CH:21]([CH3:23])[CH3:22])=[O:9])[CH2:4][CH2:3]1.C(N(CC)CC)C.[CH3:31][S:32](Cl)(=[O:34])=[O:33]>ClCCl>[CH:21]([O:20][C:11]1[CH:12]=[CH:13][C:14]([S:16]([CH3:19])(=[O:18])=[O:17])=[CH:15][C:10]=1[C:8]([N:5]1[CH2:4][CH2:3][CH:2]([O:1][S:32]([CH3:31])(=[O:34])=[O:33])[CH2:7][CH2:6]1)=[O:9])([CH3:23])[CH3:22]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 58673083(4-Hydroxy-piperidin-1-yl)-(2-isopropoxy-5-methanesulfonyl-phenyl)-methanone

생성물 1

HCID 58673076Methanesulfonic acid 1-(2-isopropoxy-5-methanesulfonyl-benzoyl)-piperidin-4-yl ester수율 93%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

반응 조건

온도
0 °C

실험 절차

To a solution of 0.29 mmol (4-hydroxy-piperidin-1-yl)-(2-isopropoxy-5-methanesulfonyl-phenyl)-methanone in 6 ml dichloromethane at 0° C. were added successively 0.73 mmol triethylamine and 0.35 mmol methanesulfonyl chloride. The reaction mixture was stirred at 0° C. for 20 min and then at RT for 2 h. The reaction mixture was then diluted with dichloromethane, washed with water, and the organic phase dried over sodium sulfate and concentrated in vacuo to afford the title compound as a light brown solid (yield 93%). MS (m/e): 420.1 (M+H+, 100%).

후처리

  1. waitat RT for 2 h
  2. washwashed with water
  3. dry with materialthe organic phase dried over sodium sulfate
  4. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-5782904fa00043fdaaf90278f63cb018
출처 데이터셋
uspto-grants-2010_09
특허 번호
US07790763B2

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