関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | (3S,4R)-4-(4-Fluorophenyl)-3-piperidinemethanol | HCID 9855829 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | trans-(-)-4-(4-Fluorophenyl)-3-hydroxymethylpiperidine monohydrate | HCID 69039254 | 89.45% |
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
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05948914 |
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| 出典データセット | uspto-grants-1999_09 |
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| ORD ID | ord-653cfc05fa4f4689ad6b4d9b9a492ded |
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| 出典メモ | uspto-grants-1999_09 |
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