HRID31376

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 84%

AUXILIARIES

试剂、催化剂与溶剂

溶剂HCID6569

Methyl ethyl ketone

C4H8O

CONDITIONS

反应条件

温度: -5 °C

PROCEDURE

实验过程

1.5 g of levofloxacin crude was put in suspension in 15 ml of MEK. The mixture was heated to reflux temperature until complete dissolution of the material. Then the solution was cooled to −5° C. over a period of 3 hours. The precipitate was filtrated under vacuum, washed with 1.5 ml of MEK and dried at 30° C. in a vacuum oven to give 840 mg (84%) 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 1.5 ml of MEK
customdried at 30° C. in a vacuum oven

来源与证据

来源类型: Open Reaction Database
ORD 记录: ord-5ef30b4014b14c6b9ef8a9cf7daa197a
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>CCC(C)=O>[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]