HRID2090525

反应详情

EQUATION

反应方程式

REACTANTS

反应物

HCID444972

Fumaric acid

C4H4O4

结构：Cc1ccc(S(=O)(=O)[O-])cc1.NC(=O)c1cccc2cn(-c3ccc([C@@H]4CCC[NH2+]C4)cc3)nc12

HCID44137083

未命名化合物

PRODUCTS

生成物

结构：NC(=O)c1cccc2cn(-c3ccc([C@@H]4CCC[NH2+]C4)cc3)nc12.NC(=O)c1cccc2cn(-c3ccc([C@@H]4CCC[NH2+]C4)cc3)nc12.O=C([O-])/C=C/C(=O)[O-]

HCID68771419

未命名化合物

AUXILIARIES

试剂、催化剂与溶剂

溶剂HCID702

Ethanol

C2H6O

CONDITIONS

反应条件

温度: 40 °C

PROCEDURE

实验过程

50 mg of tert-butyl(3S)-3-{4-[7-(aminocarbonyl)-2H-indazol-2-yl]phenyl}piperidine-1-carboxylate (Example 1, D3) as a compound stock solution was reacted with 1 mole equivalent of fumaric acid, added as a 0.405 Molar solution in ethanol. Excess solvent was removed under centrifugal evaporation and 1 mL of ethanol added at ambient room temperature (˜25° C.). The resultant solution stirred at 40° C. for 24 hours. The experiment was left to gently evaporate under atmospheric conditions where a colorless solid was observed. This solid was analyzed using x-ray powder diffraction, proton NMR, DSC and TGA to confirm the formation of the title salt.

WORKUP

后处理

customExcess solvent was removed under centrifugal evaporation and 1 mL of ethanol
additionadded at ambient room temperature (˜25° C.)
waitThe experiment was left
customto gently evaporate under atmospheric conditions where a colorless solid

来源与证据

来源类型: Open Reaction Database
ORD 记录: ord-6a35c0bfec054d4398451050c4b957fa
来源数据集: uspto-grants-2013_05
DOI: 10.6084/m9.figshare.5104873.v1
专利: US08436185B2
来源说明: uspto-grants-2013_05

反应 SMILES

CC1C=CC(S([O-])(=O)=O)=CC=1.[NH2:12][C:13]([C:15]1[C:23]2[C:19](=[CH:20][N:21]([C:24]3[CH:29]=[CH:28][C:27]([C@@H:30]4[CH2:35][CH2:34][CH2:33][NH2+:32][CH2:31]4)=[CH:26][CH:25]=3)[N:22]=2)[CH:18]=[CH:17][CH:16]=1)=[O:14].[C:36]([OH:43])(=[O:42])/[CH:37]=[CH:38]/[C:39]([OH:41])=[O:40]>C(O)C>[C:36]([O-:43])(=[O:42])/[CH:37]=[CH:38]/[C:39]([O-:41])=[O:40].[NH2:12][C:13]([C:15]1[C:23]2[C:19](=[CH:20][N:21]([C:24]3[CH:29]=[CH:28][C:27]([C@@H:30]4[CH2:35][CH2:34][CH2:33][NH2+:32][CH2:31]4)=[CH:26][CH:25]=3)[N:22]=2)[CH:18]=[CH:17][CH:16]=1)=[O:14].[NH2:12][C:13]([C:15]1[C:23]2[C:19](=[CH:20][N:21]([C:24]3[CH:29]=[CH:28][C:27]([C@@H:30]4[CH2:35][CH2:34][CH2:33][NH2+:32][CH2:31]4)=[CH:26][CH:25]=3)[N:22]=2)[CH:18]=[CH:17][CH:16]=1)=[O:14]