HRID31371

反应详情

EQUATION

反应方程式

REACTANTS

反应物

结构：C[C@H]1COc2c(N3CCN(C)CC3)c(F)cc3c(=O)c(C(=O)O)cn1c23

HCID149096

Levofloxacin

C18H20FN3O4

PRODUCTS

生成物

结构：C[C@H]1COc2c(N3CCN(C)CC3)c(F)cc3c(=O)c(C(=O)O)cn1c23.C[C@H]1COc2c(N3CCN(C)CC3)c(F)cc3c(=O)c(C(=O)O)cn1c23.O

HCID3033924

Levofloxacin hydrate

C36H42F2N6O9

收率 118.5%

AUXILIARIES

试剂、催化剂与溶剂

溶剂HCID263

1-Butanol

C4H10O

PROCEDURE

实验过程

1 g of levofloxacin crude was put in suspension in 7 ml of n-BuOH. The mixture was heated to reflux temperature until complete dissolution of the material. Then the solution was cooled to RT over a period of 2.5 hours. The precipitate was filtrated under vacuum, washed with n-BuOH and dried at 60° C. in a vacuum oven to give 810 mg (81%) of purified levofloxacin hemihydrate.

WORKUP

后处理

temperatureThe mixture was heated
temperatureto reflux temperature
dissolutionuntil complete dissolution of the material
filtrationThe precipitate was filtrated under vacuum
washwashed with n-BuOH
customdried at 60° C. in a vacuum oven

来源与证据

来源类型: Open Reaction Database
ORD 记录: ord-edc8959a3ec14e8e9a416f73ba49e7be
来源数据集: uspto-grants-2008_09
DOI: 10.6084/m9.figshare.5104873.v1
专利: US07425628B2
来源说明: uspto-grants-2008_09

反应 SMILES

[CH3:1][C@@H:2]1[N:23]2[C:6]3[C:7]([C:19]([C:21]([C:24]([OH:26])=[O:25])=[CH:22]2)=[O:20])=[CH:8][C:9]([F:18])=[C:10]([N:11]2[CH2:16][CH2:15][N:14]([CH3:17])[CH2:13][CH2:12]2)[C:5]=3[O:4][CH2:3]1>CCCCO>[CH3:1][C@@H:2]1[N:23]2[CH:22]=[C:21]([C:24]([OH:26])=[O:25])[C:19]([C:7]3=[CH:8][C:9]([F:18])=[C:10]([N:11]4[CH2:16][CH2:15][N:14]([CH3:17])[CH2:13][CH2:12]4)[C:5](=[C:6]23)[O:4][CH2:3]1)=[O:20].[CH3:1][C@@H:2]1[N:23]2[CH:22]=[C:21]([C:24]([OH:26])=[O:25])[C:19]([C:7]3=[CH:8][C:9]([F:18])=[C:10]([N:11]4[CH2:16][CH2:15][N:14]([CH3:17])[CH2:13][CH2:12]4)[C:5](=[C:6]23)[O:4][CH2:3]1)=[O:20].[OH2:4]