HRID553430

反应详情

EQUATION

反应方程式

REACTANTS

反应物

结构：Cc1ccc(NC(=O)c2ccc(CN3CCN(C)CC3)cc2)cc1Nc1nccc(-c2cccnc2)n1

HCID5291

Imatinib

C29H31N7O

HCID6395

Methanesulfonic acid

CH4O3S

PRODUCTS

生成物

结构：CS(=O)(=O)O.Cc1ccc(NC(=O)c2ccc(CN3CCN(C)CC3)cc2)cc1Nc1nccc(-c2cccnc2)n1

HCID123596

Imatinib mesylate

C30H35N7O4S

AUXILIARIES

试剂、催化剂与溶剂

溶剂HCID702

Ethanol

C2H6O

PROCEDURE

实验过程

Imatinib base was suspended in ethanol, methane sulfonic acid was added and heated under reflux for 20 minutes and than filtered at 65° C. The filtrate was evaporated down to 50% and the residue filtered off at 25° C. (filter material A). The mother liquor was evaporated to dryness. The residue and filter material A were suspended in ethanol dissolved under reflux with addition of water. Cooling overnight to 25° C., filtration and drying yielded Imatinib mesylate α-crystal form.

WORKUP

后处理

temperatureheated
temperatureunder reflux for 20 minutes
filtrationthan filtered at 65° C
customThe filtrate was evaporated down to 50%
filtrationthe residue filtered off at 25° C.
filtration(filter material A)
customThe mother liquor was evaporated to dryness
filtrationThe residue and filter material A
dissolutiondissolved
temperatureunder reflux with addition of water
temperatureCooling
filtrationovernight to 25° C., filtration
customdrying

来源与证据

来源类型: Open Reaction Database
ORD 记录: ord-5cc0358765cf4de4956c0e8344c30b49
来源数据集: uspto-grants-2011_11
DOI: 10.6084/m9.figshare.5104873.v1
专利: US08048883B2
来源说明: uspto-grants-2011_11

反应 SMILES

[CH3:1][C:2]1[CH:3]=[CH:4][C:5]([NH:21][C:22]([C:24]2[CH:25]=[CH:26][C:27]([CH2:30][N:31]3[CH2:36][CH2:35][N:34]([CH3:37])[CH2:33][CH2:32]3)=[CH:28][CH:29]=2)=[O:23])=[CH:6][C:7]=1[NH:8][C:9]1[N:10]=[CH:11][CH:12]=[C:13]([C:15]2[CH:16]=[CH:17][CH:18]=[N:19][CH:20]=2)[N:14]=1.[CH3:38][S:39]([OH:42])(=[O:41])=[O:40]>C(O)C>[CH3:1][C:2]1[CH:3]=[CH:4][C:5]([NH:21][C:22]([C:24]2[CH:29]=[CH:28][C:27]([CH2:30][N:31]3[CH2:32][CH2:33][N:34]([CH3:37])[CH2:35][CH2:36]3)=[CH:26][CH:25]=2)=[O:23])=[CH:6][C:7]=1[NH:8][C:9]1[N:10]=[CH:11][CH:12]=[C:13]([C:15]2[CH:16]=[CH:17][CH:18]=[N:19][CH:20]=2)[N:14]=1.[CH3:38][S:39]([OH:42])(=[O:41])=[O:40]