Acetone → Erythromycin

HRID 2090141

反応式

HRID 2090141 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.CC(C)=O>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

4

反応物 2

HCID 180AcetoneHCID 83938Erythromycin Thiocyanate

生成物 1

HCID 12560Erythromycin収率 15%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

反応条件

温度
34 °C

実験手順

A mixture of erythromycin thiocyanate and other impurities (100 g) was added into a solvent mixture (300 mL) comprising dichloromethane and acetone (the volume content of dichloromethane is 60%), stirred under heat to 34° 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 15% of erythromycin A. The dichloromethane solution was cooled to 23° C., kept for one hour and then cooled to 3° C. in 16 hours. The crystals formed were filtered. Dichloromethane (20 mL) (the content of dichloromethane is 95% and ethanol is 5%) was used to wash the crystals and the crystals were filtered for further 5 minutes. The amount of erythromycin A in the dried erythromycin is 94.6% with a dichloromethane content of 352 ppm, a water content of 2.2% and a microbiological titre of 941 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-c9bdf1dbb5f7473cbb54edd3d6cee7b4
出典データセット
uspto-grants-2013_05
特許番号
US08436154B2

関連ノート

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