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HRID 617440作成日:2026年10月25日

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

https://huagongshe.com/reaction/617440

反応式

関与物質

役割名称HCID仕込み量
反応物WaterHCID 962—
反応物(3S,4R)-4-(4-Fluorophenyl)-3-piperidinemethanolHCID 9855829—
溶媒TolueneHCID 1140—
生成物trans-(-)-4-(4-Fluorophenyl)-3-hydroxymethylpiperidine monohydrateHCID 6903925489.45%

反応手順

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.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US05948914
出典データセットuspto-grants-1999_09
ORD IDord-653cfc05fa4f4689ad6b4d9b9a492ded
出典メモuspto-grants-1999_09