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

HRID 128213

반응식

HRID 128213 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매2회

실험 절차

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.

후처리

  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.

출처 및 근거

ORD 기록
ord-3082894a3de041108a4101f472094825
출처 데이터셋
uspto-grants-1981_03
특허 번호
US04259329

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