HRID2039872

反应详情

EQUATION

反应方程式

REACTANTS

反应物

HCID311

Citric acid

C6H8O7

HCID6329

Methylamine

CH5N

结构：COC(=O)CC1CN(C(=O)c2c(Oc3c(C)cccc3C)n(-c3ccccc3)c3cccnc23)CCN1C(=O)OC(C)(C)C

HCID66922257

未命名化合物

PRODUCTS

生成物

结构：CNC(=O)CC1CN(C(=O)c2c(Oc3c(C)cccc3C)n(-c3ccccc3)c3cccnc23)CCN1C(=O)OC(C)(C)C

HCID66922143

未命名化合物

收率 32.2%

CONDITIONS

反应条件

温度: 40 °C

PROCEDURE

实验过程

A solution of the crude compound of example 58, step 2, (140 mg, 234 μmol) in MOH (1 ml) was mixed with a 2 M methanolic solution of methylamine (2.60 ml, 5.19 mmol). The reaction mixture was stirred at 40° C. for 7 days. After cooling to room temperature, the mixture was neutralized with an aqueous solution of citric acid and extracted with EA. The combined organic phases were dried over sodium sulfate and evaporated. 45 mg of crude title compound were obtained.

WORKUP

后处理

temperatureAfter cooling to room temperature
extractionextracted with EA
dry with materialThe combined organic phases were dried over sodium sulfate
customevaporated

来源与证据

来源类型: Open Reaction Database
ORD 记录: ord-d8d5542763a64eae8fc588d2c024ea97
来源数据集: uspto-grants-2013_11
DOI: 10.6084/m9.figshare.5104873.v1
专利: US08580813B2
来源说明: uspto-grants-2013_11

反应 SMILES

[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][N:11]([C:14]([C:16]2[C:20]3=[N:21][CH:22]=[CH:23][CH:24]=[C:19]3[N:18]([C:25]3[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=3)[C:17]=2[O:31][C:32]2[C:37]([CH3:38])=[CH:36][CH:35]=[CH:34][C:33]=2[CH3:39])=[O:15])[CH2:10][CH:9]1[CH2:40][C:41]([O:43]C)=O)=[O:7])([CH3:4])([CH3:3])[CH3:2].[CH3:45][NH2:46].C(O)(=O)CC(CC(O)=O)(C(O)=O)O>>[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][N:11]([C:14]([C:16]2[C:20]3=[N:21][CH:22]=[CH:23][CH:24]=[C:19]3[N:18]([C:25]3[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=3)[C:17]=2[O:31][C:32]2[C:33]([CH3:39])=[CH:34][CH:35]=[CH:36][C:37]=2[CH3:38])=[O:15])[CH2:10][CH:9]1[CH2:40][C:41](=[O:43])[NH:46][CH3:45])=[O:7])([CH3:2])([CH3:3])[CH3:4]