HRID916790

反应详情

EQUATION

反应方程式

REACTANTS

反应物

HCID31297

Methanesulfonyl chloride

CH3ClO2S

结构：Nc1ncnc2c1c(C(=O)c1cccc(NC(=O)Nc3cc(Cl)cc(Cl)c3)c1)cn2C1CCNCC1

HCID67219862

未命名化合物

PRODUCTS

生成物

结构：CS(=O)(=O)N1CCC(n2cc(C(=O)c3cccc(NC(=O)Nc4cc(Cl)cc(Cl)c4)c3)c3c(N)ncnc32)CC1

HCID67218832

未命名化合物

收率 19%

AUXILIARIES

试剂、催化剂与溶剂

溶剂HCID22350042

未命名化合物

PROCEDURE

实验过程

A solution of 1-[3-(4-Amino-7-piperidin-4-yl-7H-pyrrolo[2,3-d]pyrimidine-5-carbonyl)-phenyl]-3-(3,5-dichloro-phenyl)-urea (100 mg, 0.19 mmol) and methanesulfonylchloride (22 mg, 0.19 mmol) in DMF/CH2Cl2 (2/3, 5 mL) was stirred in a sealed tube for 1.5 hours at room temperature. The reaction mixture concentrated in vacuo. Purification by reverse phase preparative HPLC (HPLC method 2) provided the title compound as a white solid (21.8 mg, 19%). MS: 603.5 (MH+); HPLC Rf: 2.3 min. (HPLC method 2); HPLC purity: 100%.

WORKUP

后处理

concentrationThe reaction mixture concentrated in vacuo
customPurification by reverse phase preparative HPLC (HPLC method 2)

来源与证据

来源类型: Open Reaction Database
ORD 记录: ord-fc6577b2e84144dca34199561fe47c15
来源数据集: uspto-grants-2007_09
DOI: 10.6084/m9.figshare.5104873.v1
专利: US07271262B2
来源说明: uspto-grants-2007_09

反应 SMILES

[NH2:1][C:2]1[C:3]2[C:10]([C:11]([C:13]3[CH:14]=[C:15]([NH:19][C:20]([NH:22][C:23]4[CH:28]=[C:27]([Cl:29])[CH:26]=[C:25]([Cl:30])[CH:24]=4)=[O:21])[CH:16]=[CH:17][CH:18]=3)=[O:12])=[CH:9][N:8]([CH:31]3[CH2:36][CH2:35][NH:34][CH2:33][CH2:32]3)[C:4]=2[N:5]=[CH:6][N:7]=1.[CH3:37][S:38](Cl)(=[O:40])=[O:39]>CN(C=O)C.C(Cl)Cl>[NH2:1][C:2]1[C:3]2[C:10]([C:11]([C:13]3[CH:14]=[C:15]([NH:19][C:20]([NH:22][C:23]4[CH:28]=[C:27]([Cl:29])[CH:26]=[C:25]([Cl:30])[CH:24]=4)=[O:21])[CH:16]=[CH:17][CH:18]=3)=[O:12])=[CH:9][N:8]([CH:31]3[CH2:32][CH2:33][N:34]([S:38]([CH3:37])(=[O:40])=[O:39])[CH2:35][CH2:36]3)[C:4]=2[N:5]=[CH:6][N:7]=1