D-Tartaric acid → 17-Cyclobutylmethyl-3-hydroxy-8beta-methylmorphinan-6-one Tartrate

HRID 128213

反応式

HRID 128213 の反応式
[C:1]([OH:10])(=[O:9])[C@H:2]([C@@H:4]([C:6]([OH:8])=[O:7])[OH:5])[OH:3].[CH:11]1([CH2:15][N:16]2[CH2:33][CH2:32][C@@:23]34[C:24]5[CH:25]=[C:26]([OH:31])[CH:27]=[CH:28][C:29]=5[CH2:30][C@@H:17]2[C@@H:18]3[C@@H:19]([CH3:35])[CH2:20][C:21](=[O:34])[CH2:22]4)[CH2:14][CH2:13][CH2:12]1>C(O)C>[C:6]([CH:4]([CH:2]([C:1]([OH:10])=[O:9])[OH:3])[OH:5])([OH:8])=[O:7].[CH:11]1([CH2:15][N:16]2[CH2:33][CH2:32][C@@:23]34[C:24]5[CH:25]=[C:26]([OH:31])[CH:27]=[CH:28][C:29]=5[CH2:30][C@@H:17]2[C@@H:18]3[C@@H:19]([CH3:35])[CH2:20][C:21](=[O:34])[CH2:22]4)[CH2:14][CH2:13][CH2:12]1

参加物

4

反応物 2

HCID 439655D-Tartaric acidHCID 5388867717-Cyclobutylmethyl-3-hydroxy-8beta-methylmorphinan-6-one

生成物 1

HCID 7052884217-Cyclobutylmethyl-3-hydroxy-8beta-methylmorphinan-6-one Tartrate

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒2 回

実験手順

To a stirred solution of d-tartaric acid (16.09, 106 mmole) in ethanol (100 ml) was added dropwise a solution of 17-cyclobutylmethyl-3-hydroxy-8β-methylmorphinan-6-one (TR-5130-free base, 32.0 g, 94 mmole) in ethanol (100 ml). After several minutes of stirring, a white solid began to precipitate. The slurry was stirred at room temperature for several hours and then kept in the cold overnight. The solid was collected, washed with cold ethanol followed by ether and dried at atmospheric pressure and 115° C. for one hour to give 32.0 g (69%) of TR-5257 as a white powder, mp. 210°-213° dec.

後処理

  1. customto precipitate
  2. stirringThe slurry was stirred at room temperature for several hours
  3. customkept in the cold overnight
  4. customThe solid was collected
  5. washwashed with cold ethanol
  6. customdried at atmospheric pressure and 115° C. for one hour
  7. customto give 32.0 g (69%) of TR-5257 as a white powder, mp. 210°-213° dec.

出典と根拠

ORDレコード
ord-3082894a3de041108a4101f472094825
出典データセット
uspto-grants-1981_03
特許番号
US04259329

関連ノート

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