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

HRID 1016676ノート

反応式

HRID 1016676 の反応式
[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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-8e4e9f87089c46f1b9f46d2e3df1680d
出典データセット
uspto-grants-2002_11
特許番号
US06476227B1

反応ノート

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