HRID1184283

反应详情

EQUATION

反应方程式

REACTANTS

反应物

HCID6395

Methanesulfonic acid

CH4O3S

HCID8058

n-Hexane

C6H14

结构：COCCCCn1c(C(=O)N(CC(C)C)[C@@H]2CNC[C@H](C(=O)N3CCOCC3)C2)nc2ccccc21

HCID44554894

未命名化合物

PRODUCTS

生成物

结构：COCCCCn1c(C(=O)N(CC(C)C)[C@@H]2CNC[C@H](C(=O)N3CCOCC3)C2)nc2ccccc21.CS(=O)(=O)O

HCID86642216

未命名化合物

AUXILIARIES

试剂、催化剂与溶剂

溶剂HCID8857

Ethyl acetate

C4H8O2

2 次

PROCEDURE

实验过程

1-(4-Methoxybutyl)-N-(2-methylpropyl)-N-[(3S,5R)-5-(morpholin-4-ylcarbonyl)piperidin-3-yl]-1H-benzimidazole-2-carboxamide (208 mg) was dissolved in ethyl acetate (2 ml), a solution of methanesulfonic acid (40 μl) in ethyl acetate (1 ml) was added at 75° C., hexane (1 ml) was added, and the mixture was heated under reflux and stood at room temperature overnight. The precipitated crystals were collected by filtration, and dried at 70° C. for 3 hr to give the object product (158 mg).

WORKUP

后处理

temperaturethe mixture was heated
temperatureunder reflux
filtrationThe precipitated crystals were collected by filtration
customdried at 70° C. for 3 hr

来源与证据

来源类型: Open Reaction Database
ORD 记录: ord-19009ba7fb0b4cbd8400c56af6f2c6ed
来源数据集: uspto-grants-2014_03
DOI: 10.6084/m9.figshare.5104873.v1
专利: US08664380B2
来源说明: uspto-grants-2014_03

反应 SMILES

[CH3:1][O:2][CH2:3][CH2:4][CH2:5][CH2:6][N:7]1[C:11]2[CH:12]=[CH:13][CH:14]=[CH:15][C:10]=2[N:9]=[C:8]1[C:16]([N:18]([CH2:33][CH:34]([CH3:36])[CH3:35])[C@H:19]1[CH2:24][C@@H:23]([C:25]([N:27]2[CH2:32][CH2:31][O:30][CH2:29][CH2:28]2)=[O:26])[CH2:22][NH:21][CH2:20]1)=[O:17].[CH3:37][S:38]([OH:41])(=[O:40])=[O:39].CCCCCC>C(OCC)(=O)C>[CH3:37][S:38]([OH:41])(=[O:40])=[O:39].[CH3:1][O:2][CH2:3][CH2:4][CH2:5][CH2:6][N:7]1[C:11]2[CH:12]=[CH:13][CH:14]=[CH:15][C:10]=2[N:9]=[C:8]1[C:16]([N:18]([CH2:33][CH:34]([CH3:36])[CH3:35])[C@H:19]1[CH2:24][C@@H:23]([C:25]([N:27]2[CH2:32][CH2:31][O:30][CH2:29][CH2:28]2)=[O:26])[CH2:22][NH:21][CH2:20]1)=[O:17]