HRID1470524

反应详情

EQUATION

反应方程式

REACTANTS

反应物

HCID11430

Potassium Carbonate

CK2O3

HCID22466

Carbonochloridic acid, hexyl ester

C7H13ClO2

结构：CCOC(=O)CCN(C(=O)c1ccc2c(c1)nc(CNc1ccc(C(=N)N)cc1)n2C)c1ccccn1.Cc1ccc(S(=O)(=O)O)cc1

HCID16202315

β-Alanine, N-[[2-[[[4-(aminoiminomethyl)phenyl]amino]methyl]-1-methyl-1H-benzimidazol-5-yl]carbonyl]-N-2-pyridinyl-, ethyl ester, 4-methylbenzenesulfonate (1:1)

C34H37N7O6S

PRODUCTS

生成物

$结构：CCCCCCOC(=O)/N=C(\N)c1ccc(NCc2nc3cc(C(=O)N(CCC(=O)OCC)c4ccccn4)ccc3n2C)cc1$

HCID6445226

未命名化合物

AUXILIARIES

试剂、催化剂与溶剂

溶剂HCID180

Acetone

C3H6O

溶剂HCID962

Water

H2O

PROCEDURE

实验过程

55 g of 1-methyl-2-[N-[4-amidinophenyl]aminomethyl]benzimidazol-5-yl carboxylic acid-N-(2-pyridyl)-N-(2-ethoxycarbonylethyl)amide tosylate was dissolved in 437 ml of acetone and 273 ml of water. 16.4 g of hexyl chloroformate and 34 g of potassium carbonate was added to it at a temperature of about 15° C. After the end of the reaction, the precipitated product is filtered off and washed with acetone/water. Dissolved the obtained solid in 270 ml of acetone under heating and then filtered. The title product was crystallized by the addition of 220 ml of water. The isolated substance is dried under reduced pressure at 45° C.

WORKUP

后处理

customAfter the end of the reaction
filtrationthe precipitated product is filtered off
washwashed with acetone/water
dissolutionDissolved the obtained solid in 270 ml of acetone
temperatureunder heating
filtrationfiltered
customThe title product was crystallized by the addition of 220 ml of water
customThe isolated substance is dried under reduced pressure at 45° C.

来源与证据

来源类型: Open Reaction Database
ORD 记录: ord-c51b1cda867140ca90bcb5001b84285c
来源数据集: uspto-grants-2015_04
DOI: 10.6084/m9.figshare.5104873.v1
专利: US09006448B2
来源说明: uspto-grants-2015_04

反应 SMILES

S(C1C=CC(C)=CC=1)(O)(=O)=O.[N:12]1[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=1[N:18]([CH2:42][CH2:43][C:44]([O:46][CH2:47][CH3:48])=[O:45])[C:19]([C:21]1[CH:41]=[CH:40][C:24]2[N:25]([CH3:39])[C:26]([CH2:28][NH:29][C:30]3[CH:35]=[CH:34][C:33]([C:36](=[NH:38])[NH2:37])=[CH:32][CH:31]=3)=[N:27][C:23]=2[CH:22]=1)=[O:20].Cl[C:50]([O:52][CH2:53][CH2:54][CH2:55][CH2:56][CH2:57][CH3:58])=[O:51].C(=O)([O-])[O-].[K+].[K+]>CC(C)=O.O>[CH3:58][CH2:57][CH2:56][CH2:55][CH2:54][CH2:53][O:52][C:50](/[N:38]=[C:36](\[NH2:37])/[C:33]1[CH:32]=[CH:31][C:30]([NH:29][CH2:28][C:26]2[N:25]([CH3:39])[C:24]3[CH:40]=[CH:41][C:21]([C:19]([N:18]([C:13]4[CH:14]=[CH:15][CH:16]=[CH:17][N:12]=4)[CH2:42][CH2:43][C:44]([O:46][CH2:47][CH3:48])=[O:45])=[O:20])=[CH:22][C:23]=3[N:27]=2)=[CH:35][CH:34]=1)=[O:51]