HRID222969

反应详情

EQUATION

反应方程式

REACTANTS

反应物

HCID6101

4-Methylbenzenesulfonic acid

C7H8O3S

结构：Cc1ccc(NC(=O)c2ccsc2)cc1-c1nc(NC2CC(C)(C)NC(C)(C)C2)nc2c1ccc(=O)n2-c1c(F)cccc1F

HCID11947981

未命名化合物

PRODUCTS

生成物

结构：Cc1ccc(NC(=O)c2ccsc2)cc1-c1nc(NC2CC(C)(C)NC(C)(C)C2)nc2c1ccc(=O)n2-c1c(F)cccc1F.Cc1ccc(S(=O)(=O)O)cc1

HCID86608568

未命名化合物

AUXILIARIES

试剂、催化剂与溶剂

溶剂HCID3776

Isopropanol

C3H8O

CONDITIONS

反应条件

温度: 60 °C

PROCEDURE

实验过程

Added IPA (5 mL) to N-(3-{8-(2,6-difluorophenyl)-7-oxo-2-[(2,2,6,6-tetramethyl-4-piperidinyl)amino]-7,8-dihydropyrido[2,3-d]pyrimidin-4-yl}-4-methylphenyl)-3-thiophenecarboxamide (203.2 mg) and heated to 60° C. Added p-toluenesulfonic acid (1.1 eq; 1M in water), and solution clarified. After a few minutes at about 60° C., cooled to rt. Stirred for about 3 hrs at rt, then filtered, washed with IPA, and dried in vacuum oven at 50° C. to provide the title compound (123.9 mg). Melting point (tested with DSC) is 335° C.

WORKUP

后处理

waitAfter a few minutes at about 60° C.
temperaturecooled to rt
filtrationfiltered
washwashed with IPA
customdried in vacuum oven at 50° C.

来源与证据

来源类型: Open Reaction Database
ORD 记录: ord-5ff8030c943240fa8cf549d841770d94
来源数据集: uspto-grants-2012_06
DOI: 10.6084/m9.figshare.5104873.v1
专利: US08207176B2
来源说明: uspto-grants-2012_06

反应 SMILES

[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([F:8])[C:3]=1[N:9]1[C:14]2[N:15]=[C:16]([NH:34][CH:35]3[CH2:40][C:39]([CH3:42])([CH3:41])[NH:38][C:37]([CH3:44])([CH3:43])[CH2:36]3)[N:17]=[C:18]([C:19]3[CH:20]=[C:21]([NH:26][C:27]([C:29]4[CH:33]=[CH:32][S:31][CH:30]=4)=[O:28])[CH:22]=[CH:23][C:24]=3[CH3:25])[C:13]=2[CH:12]=[CH:11][C:10]1=[O:45].[C:46]1([CH3:56])[CH:51]=[CH:50][C:49]([S:52]([OH:55])(=[O:54])=[O:53])=[CH:48][CH:47]=1>CC(O)C>[CH3:56][C:46]1[CH:47]=[CH:48][C:49]([S:52]([OH:55])(=[O:54])=[O:53])=[CH:50][CH:51]=1.[F:8][C:4]1[CH:5]=[CH:6][CH:7]=[C:2]([F:1])[C:3]=1[N:9]1[C:14]2[N:15]=[C:16]([NH:34][CH:35]3[CH2:36][C:37]([CH3:43])([CH3:44])[NH:38][C:39]([CH3:42])([CH3:41])[CH2:40]3)[N:17]=[C:18]([C:19]3[CH:20]=[C:21]([NH:26][C:27]([C:29]4[CH:33]=[CH:32][S:31][CH:30]=4)=[O:28])[CH:22]=[CH:23][C:24]=3[CH3:25])[C:13]=2[CH:12]=[CH:11][C:10]1=[O:45]