Water → trans-(-)-4-(4-Fluorophenyl)-3-hydroxymethylpiperidine monohydrate

HRID 1016676

반응식

HRID 1016676 반응식
[F:1][C:2]1[CH:7]=[CH:6][C:5]([C@@H:8]2[CH2:13][CH2:12][NH:11][CH2:10][C@H:9]2[CH2:14][OH:15])=[CH:4][CH:3]=1.O>C1(C)C=CC=CC=1>[OH2:15].[F:1][C:2]1[CH:7]=[CH:6][C:5]([C@@H:8]2[CH2:13][CH2:12][NH:11][CH2:10][C@H:9]2[CH2:14][OH:15])=[CH:4][CH:3]=1

참가 물질

4

반응물 2

HCID 962WaterHCID 9855829(3S,4R)-4-(4-Fluorophenyl)-3-piperidinemethanol

생성물 1

HCID 69039254trans-(-)-4-(4-Fluorophenyl)-3-hydroxymethylpiperidine monohydrate수율 89.45%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

A 200-ml four-necked glass flask equipped with a thermometer and a reflux condenser was charged with 63 ml of toluene and 10.54 g (50.37 mmol) of (−)-(3S,4R)-4-(4-fluorophenyl)-3-hydroxymethylpiperidine, and the mixture was warmed and dissolved. 1.13 g (62.71 mmol) of water was added to the above mixture at 50° C. to allow to crystallize. Thereafter, the mixture was kept for one hour at a temperature of from 20° to 30° C., and then the crystals were collected by filtration. The obtained crystals were thoroughly washed with 20 ml of toluene, to give white crystals of (−)-(3S,4R)-4-(4-fluorophenyl)-3-hydroxymethylpiperidine monohydrate. Thereafter, the crystals were dried under a reduced pressure at a temperature of 30° C. or lower, and weighed 10.24 g. The yield was 89.45% based on (−)-(3S,4R)-4-(4-fluorophenyl)-3-hydroxymethylpiperidine.

후처리

  1. customA 200-ml four-necked glass flask equipped with a thermometer and a reflux condenser
  2. temperaturethe mixture was warmed
  3. dissolutiondissolved
  4. customto crystallize
  5. filtrationthe crystals were collected by filtration
  6. washThe obtained crystals were thoroughly washed with 20 ml of toluene

출처 및 근거

ORD 기록
ord-8e4e9f87089c46f1b9f46d2e3df1680d
출처 데이터셋
uspto-grants-2002_11
특허 번호
US06476227B1

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