HRID1503318

反应详情

EQUATION

反应方程式

REACTANTS

反应物

HCID15413

Methyl tert-butyl ether

C5H12O

结构：Cc1c(-c2ccc(O)cc2)n(Cc2ccc(OCCN3CCCCCC3)cc2)c2ccc(O)cc12

HCID154257

Bazedoxifene

C30H34N2O3

PRODUCTS

生成物

结构：CC(=O)O.Cc1c(-c2ccc(O)cc2)n(Cc2ccc(OCCN3CCCCCC3)cc2)c2ccc(O)cc12

HCID154256

Bazedoxifene acetate

C32H38N2O5

AUXILIARIES

试剂、催化剂与溶剂

溶剂HCID176

Acetic Acid

C2H4O2

PROCEDURE

实验过程

Bazedoxifene free base (400 mg) and methyl tert-butyl ether (30 mL) are mixed and stirred for about 10 minutes. Acetic acid (0.17 g) is added slowly through a dropper and the mixture is stirred overnight for solid formation. The solid is collected by filtration to afford 250 mg of crystalline bazedoxifene acetate Form D.

WORKUP

后处理

stirringthe mixture is stirred overnight for solid formation
filtrationThe solid is collected by filtration

来源与证据

来源类型: Open Reaction Database
ORD 记录: ord-b6ac894438f44dbcbe6c1b754deae012
来源数据集: uspto-grants-2015_12
DOI: 10.6084/m9.figshare.5104873.v1
专利: US09212172B2
来源说明: uspto-grants-2015_12

反应 SMILES

[CH3:1][C:2]1[C:3]2[CH:4]=[C:5]([OH:35])[CH:6]=[CH:7][C:8]=2[N:9]([CH2:18][C:19]2[CH:20]=[CH:21][C:22]([O:25][CH2:26][CH2:27][N:28]3[CH2:34][CH2:33][CH2:32][CH2:31][CH2:30][CH2:29]3)=[CH:23][CH:24]=2)[C:10]=1[C:11]1[CH:12]=[CH:13][C:14]([OH:17])=[CH:15][CH:16]=1.[C:36]([O:40]C)([CH3:39])(C)C>C(O)(=O)C>[CH3:1][C:2]1[C:3]2[CH:4]=[C:5]([OH:35])[CH:6]=[CH:7][C:8]=2[N:9]([CH2:18][C:19]2[CH:24]=[CH:23][C:22]([O:25][CH2:26][CH2:27][N:28]3[CH2:29][CH2:30][CH2:31][CH2:32][CH2:33][CH2:34]3)=[CH:21][CH:20]=2)[C:10]=1[C:11]1[CH:12]=[CH:13][C:14]([OH:17])=[CH:15][CH:16]=1.[CH3:39][C:36]([OH:40])=[O:17]