4-Benzylpiperidine → 4[-2-(4-Benzyl-piperidine-1-yl)-ethanesulfonyl]-phenol

HRID 382779

반응식

HRID 382779 반응식
Cl[CH2:2][CH2:3][S:4]([C:7]1[CH:12]=[CH:11][C:10]([OH:13])=[CH:9][CH:8]=1)(=[O:6])=[O:5].[CH2:14]([CH:21]1[CH2:26][CH2:25][NH:24][CH2:23][CH2:22]1)[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1>C(Cl)Cl>[CH2:14]([CH:21]1[CH2:26][CH2:25][N:24]([CH2:2][CH2:3][S:4]([C:7]2[CH:12]=[CH:11][C:10]([OH:13])=[CH:9][CH:8]=2)(=[O:6])=[O:5])[CH2:23][CH2:22]1)[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1

참가 물질

4

반응물 2

HCID 317384-BenzylpiperidineHCID 98132494-(2-Chloro-ethanesulfonyl)-phenol

생성물 1

HCID 97989454[-2-(4-Benzyl-piperidine-1-yl)-ethanesulfonyl]-phenol수율 38.7%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of 40.0 g 4-(2-chloro-ethanesulfonyl)-phenol (181 mmol) in 600 ml CH2Cl2 were added 69.9 g 4-benzylpiperidine (399 mmol). After stirring for 16 h at r. t. the reaction mixture was concentrated to 100 ml and directly purified by chromatography over silica gel (CH2Cl2/MeOH/NH3 19/1/0.1). Recrystallization from ethyl acetatelhexane (2:1) yielded 25 g product (70 mmol, 38%).

후처리

  1. concentrationthe reaction mixture was concentrated to 100 ml
  2. customdirectly purified by chromatography over silica gel (CH2Cl2/MeOH/NH3 19/1/0.1)
  3. customRecrystallization from ethyl acetatelhexane (2:1)

출처 및 근거

ORD 기록
ord-840af965b37549a1b786c559c48d75aa
출처 데이터셋
uspto-grants-2001_10
특허 번호
US06310213B1

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