Erythromycin Thiocyanate → Erythromycin

HRID 2090140

反応式

HRID 2090140 の反応式
[CH3:1][CH2:2][C@H:3]1[O:18][C:16](=[O:17])[C@H:15]([CH3:19])[C@@H:14]([O:20][C@@H:21]2[O:26][C@@H:25]([CH3:27])[C@H:24]([OH:28])[C@@:23]([O:30][CH3:31])([CH3:29])[CH2:22]2)[C@H:13]([CH3:32])[C@@H:12]([O:33][C@@H:34]2[O:39][C@H:38]([CH3:40])[CH2:37][C@H:36]([N:41]([CH3:43])[CH3:42])[C@H:35]2[OH:44])[C@@:11]([OH:46])([CH3:45])[CH2:10][C@@H:9]([CH3:47])[C:7](=[O:8])[C@H:6]([CH3:48])[C@@H:5]([OH:49])[C@@:4]1([OH:51])[CH3:50].C(S)#N>ClCCl>[CH3:1][CH2:2][C@H:3]1[O:18][C:16](=[O:17])[C@H:15]([CH3:19])[C@@H:14]([O:20][C@@H:21]2[O:26][C@@H:25]([CH3:27])[C@H:24]([OH:28])[C@@:23]([O:30][CH3:31])([CH3:29])[CH2:22]2)[C@H:13]([CH3:32])[C@@H:12]([O:33][C@@H:34]2[O:39][C@H:38]([CH3:40])[CH2:37][C@H:36]([N:41]([CH3:42])[CH3:43])[C@H:35]2[OH:44])[C@@:11]([OH:46])([CH3:45])[CH2:10][C@@H:9]([CH3:47])[C:7](=[O:8])[C@H:6]([CH3:48])[C@@H:5]([OH:49])[C@@:4]1([OH:51])[CH3:50]

参加物

3

反応物 1

HCID 83938Erythromycin Thiocyanate

生成物 1

HCID 12560Erythromycin収率 14%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
37 °C

実験手順

Erythromycin thiocyanate (200 g) was added into dichloromethane (500 mL), stirred under heat to 37° C. and adjusted to pH 12 until the solution became clear. The upper aqueous phase was separated and removed to obtain a dichloromethane solution with about 14% of erythromycin A. The dichloromethane solution was cooled to 24° C., kept for 2 hours and then cooled to −4° C. in 5 hours. The crystals formed were filtered. Dichloromethane (20 mL) was used to wash the crystals and the crystals were filtered for further 5 minutes. The amount of the erythromycin A in the dried erythromycin is 95.2% with a dichloromethane content of 150 ppm, a water content of 1.0% and a microbiological titre of 948 μ/mg.

後処理

  1. customThe upper aqueous phase was separated
  2. customremoved

出典と根拠

ORDレコード
ord-ae7b77708388425e8d129f7c7df6aed1
出典データセット
uspto-grants-2013_05
特許番号
US08436154B2

関連ノート

読み込み中…