HRID1876559

反应详情

EQUATION

反应方程式

REACTANTS

反应物

HCID521998

4-Methylbenzenesulfonic acid hydrate

C7H10O4S

结构：CC(=O)N1CCN(c2nc3c(N4CCOCC4)nc(-c4cnc(N)nc4)nc3n2CC(F)(F)F)C[C@H]1C

HCID45378170

未命名化合物

PRODUCTS

生成物

结构：CC(=O)N1CCN(c2nc3c(N4CCOCC4)nc(-c4cnc(N)nc4)nc3n2CC(F)(F)F)C[C@H]1C.Cc1ccc(S(=O)(=O)O)cc1

HCID86344189

未命名化合物

收率 51.6%

AUXILIARIES

试剂、催化剂与溶剂

溶剂HCID702

Ethanol

C2H6O

PROCEDURE

实验过程

To a suspension of 5-{8-[(3R)-4-acetyl-3-methylpiperazin-1-yl]-6-morpholin-4-yl-9-(2,2,2-trifluoroethyl)-9H-purin-2-yl}pyrimidin-2-amine (137 mg, 0.263 mmol) in 10% aqueous ethanol solution (2 ml) was added p-toluenesulfonic acid mono hydrate (55.2 mg, 0.290 mmol) at 50° C., and the mixture was allowed to be cooled down to room temperature, and was stirred for 3 days. The solid precipitated out was collected and dried to give 5-{8-[(3R)-4-acetyl-3-methylpiperazin-1-yl]-6-morpholin-4-yl-9-(2,2,2-trifluoroethyl)-9H-purin-2-yl}pyrimidin-2-amine p-toluenesulfonate (94 mg) as a yellow solid.

WORKUP

后处理

customThe solid precipitated out
customwas collected
customdried

来源与证据

来源类型: Open Reaction Database
ORD 记录: ord-68750757448c425e93151f9ca61f0e12
来源数据集: uspto-grants-2012_11
DOI: 10.6084/m9.figshare.5104873.v1
专利: US08309546B2
来源说明: uspto-grants-2012_11

反应 SMILES

[C:1]([N:4]1[CH2:9][CH2:8][N:7]([C:10]2[N:11]([CH2:32][C:33]([F:36])([F:35])[F:34])[C:12]3[C:17]([N:18]=2)=[C:16]([N:19]2[CH2:24][CH2:23][O:22][CH2:21][CH2:20]2)[N:15]=[C:14]([C:25]2[CH:26]=[N:27][C:28]([NH2:31])=[N:29][CH:30]=2)[N:13]=3)[CH2:6][C@H:5]1[CH3:37])(=[O:3])[CH3:2].O.[C:39]1([CH3:49])[CH:44]=[CH:43][C:42]([S:45]([OH:48])(=[O:47])=[O:46])=[CH:41][CH:40]=1>C(O)C>[C:39]1([CH3:49])[CH:40]=[CH:41][C:42]([S:45]([OH:48])(=[O:46])=[O:47])=[CH:43][CH:44]=1.[C:1]([N:4]1[CH2:9][CH2:8][N:7]([C:10]2[N:11]([CH2:32][C:33]([F:36])([F:35])[F:34])[C:12]3[C:17]([N:18]=2)=[C:16]([N:19]2[CH2:20][CH2:21][O:22][CH2:23][CH2:24]2)[N:15]=[C:14]([C:25]2[CH:26]=[N:27][C:28]([NH2:31])=[N:29][CH:30]=2)[N:13]=3)[CH2:6][C@H:5]1[CH3:37])(=[O:3])[CH3:2]