HRID1460475

反应详情

EQUATION

反应方程式

REACTANTS

反应物

$结构：O=C(O)/C=C\C(=O)O$

HCID444266

Maleic acid

C4H4O4

结构：COc1ccc(CCN2CCC[C@H]2CN2c3ccccc3CSc3ccccc32)cc1

HCID9824029

未命名化合物

PRODUCTS

生成物

$结构：COc1ccc(CCN2CCC[C@H]2CN2c3ccccc3CSc3ccccc32)cc1.O=C(O)/C=C\C(=O)O$

HCID9937325

未命名化合物

收率 64%

AUXILIARIES

试剂、催化剂与溶剂

溶剂HCID8857

Ethyl acetate

C4H8O2

2 次

PROCEDURE

实验过程

A solution of maleic acid (4.7 g) in ethyl acetate (200 ml) was added to a solution of (S)-5,11-dihydro-5-[1-(4-methoxyphenethyl)-2-pyrrolidinylmethyl]dibenzo[b,e][1,4]thiazepine (see Examples 1 and 6) (17.3 g) in ethyl acetate (100 ml) and the mixture was stirred at room temperature for 16 hours. The resulting precipitate was collected, dried and recrystallised from ethyl acetate/methanol to give the title compound as colourless crystals, (14.0 g, 64%), m.p. 153°-154° C., [α]58925 -39.7° (c=0.755 in ethanol).

WORKUP

后处理

customThe resulting precipitate was collected
customdried
customrecrystallised from ethyl acetate/methanol

来源与证据

来源类型: Open Reaction Database
ORD 记录: ord-d280254be5ce4e318aa1adc0710c1cc8
来源数据集: uspto-grants-1991_12
DOI: 10.6084/m9.figshare.5104873.v1
专利: US05071844
来源说明: uspto-grants-1991_12

反应 SMILES

[C:1]([OH:8])(=[O:7])/[CH:2]=[CH:3]\[C:4]([OH:6])=[O:5].[CH3:9][O:10][C:11]1[CH:39]=[CH:38][C:14]([CH2:15][CH2:16][N:17]2[CH2:21][CH2:20][CH2:19][C@H:18]2[CH2:22][N:23]2[C:29]3[CH:30]=[CH:31][CH:32]=[CH:33][C:28]=3[CH2:27][S:26][C:25]3[CH:34]=[CH:35][CH:36]=[CH:37][C:24]2=3)=[CH:13][CH:12]=1>C(OCC)(=O)C>[C:1]([OH:8])(=[O:7])/[CH:2]=[CH:3]\[C:4]([OH:6])=[O:5].[CH3:9][O:10][C:11]1[CH:12]=[CH:13][C:14]([CH2:15][CH2:16][N:17]2[CH2:21][CH2:20][CH2:19][C@H:18]2[CH2:22][N:23]2[C:29]3[CH:30]=[CH:31][CH:32]=[CH:33][C:28]=3[CH2:27][S:26][C:25]3[CH:34]=[CH:35][CH:36]=[CH:37][C:24]2=3)=[CH:38][CH:39]=1