HRID633672

反应详情

EQUATION

反应方程式

REACTANTS

反应物

HCID962

Water

H2O

HCID10340

Carbonic acid sodium salt (1:2)

CNa2O3

HCID4233041

3-Boc-aminopiperidine

C10H20N2O2

结构：CC(C)=CCn1c(Cl)nc2c1c(=O)n(CC(=O)c1ccccc1O)c(=O)n2C

HCID57514534

未命名化合物

PRODUCTS

生成物

结构：CC(C)=CCn1c(N2CCCC(NC(=O)OC(C)(C)C)C2)nc2c1c(=O)n(CC(=O)c1ccccc1O)c(=O)n2C

HCID66723736

未命名化合物

AUXILIARIES

试剂、催化剂与溶剂

溶剂HCID679

Dimethyl sulfoxide

C2H6OS

CONDITIONS

反应条件

温度: 60 °C

PROCEDURE

实验过程

1.30 g of 3-tert.-butyloxycarbonylamino-piperidine are added to a mixture of 2.51 g of 1-[2-(2-hydroxy-phenyl)-2-oxo-ethyl]-3-methyl-7-(3-methyl-2-buten-1-yl)-8-chloro-xanthine and 880 mg of sodium carbonate in 8 ml of dimethylsulphoxide. The reaction mixture is stirred for 18 hours at 60° C. For working up it is combined with water and the precipitate formed is suction filtered. The solid crude product is dissolved in ethyl acetate, the solution is dried over magnesium sulphate and evaporated down. The flask residue is chromatographed through a silica gel column with cyclohexane/ethyl acetate (10:1 to 1:1) as eluant.

WORKUP

后处理

customthe precipitate formed
filtrationfiltered
dissolutionThe solid crude product is dissolved in ethyl acetate
dry with materialthe solution is dried over magnesium sulphate
customevaporated down
customThe flask residue is chromatographed through a silica gel column with cyclohexane/ethyl acetate (10:1 to 1:1) as eluant

来源与证据

来源类型: Open Reaction Database
ORD 记录: ord-c48ba1d7c0ad4273ab8156db199e1727
来源数据集: uspto-grants-2016_04
DOI: 10.6084/m9.figshare.5104873.v1
专利: US09321791B2
来源说明: uspto-grants-2016_04

反应 SMILES

[C:1]([O:5][C:6]([NH:8][CH:9]1[CH2:14][CH2:13][CH2:12][NH:11][CH2:10]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].[OH:15][C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=1[C:22](=[O:42])[CH2:23][N:24]1[C:33](=[O:34])[C:32]2[N:31]([CH2:35][CH:36]=[C:37]([CH3:39])[CH3:38])[C:30](Cl)=[N:29][C:28]=2[N:27]([CH3:41])[C:25]1=[O:26].C(=O)([O-])[O-].[Na+].[Na+].O>CS(C)=O>[OH:15][C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=1[C:22](=[O:42])[CH2:23][N:24]1[C:33](=[O:34])[C:32]2[N:31]([CH2:35][CH:36]=[C:37]([CH3:38])[CH3:39])[C:30]([N:11]3[CH2:12][CH2:13][CH2:14][CH:9]([NH:8][C:6]([O:5][C:1]([CH3:4])([CH3:2])[CH3:3])=[O:7])[CH2:10]3)=[N:29][C:28]=2[N:27]([CH3:41])[C:25]1=[O:26]