HRID2363692

反应详情

EQUATION

反应方程式

REACTANTS

反应物

HCID444972

Fumaric acid

C4H4O4

结构：CC(C)c1cnn2c(NCc3ccc(-c4ccccn4)cc3)nc(NC(CO)CO)nc12

HCID46910851

未命名化合物

PRODUCTS

生成物

结构：CC(C)c1cnn2c(NCc3ccc(-c4ccccn4)cc3)nc(NC(CO)CO)nc12.O=C(O)/C=C/C(=O)O

HCID46910852

未命名化合物

AUXILIARIES

试剂、催化剂与溶剂

溶剂HCID21585056

未命名化合物

PROCEDURE

实验过程

The product 17 is treated with fumaric acid in an EtOH/Et2O solution. The fumaric acid salt 18 crystallizes from the reaction medium. Mp=179-181° C. 1H NMR (300 MHz, DMSO-d6): δ 13.11 (bs, 2H, OH), 8.76 (bs, 1H, NH), 8.64 (d, 1H, J=4.5 Hz, Harom), 8.03 (d, 2H, J=8.1 Hz, Harom), 7.94-7.82 (m, 2H, Harom), 7.72 (s, 1H, Harom) 7.49 (bs, 2H, Harom) 7.35-7.31 (m, 1H, Harom), 6.63 (s, 2H, 2 ═CH), 6.33 (d, 1H, J=6.0 Hz, NH), 4.67 (d, 2H, J=6.0 Hz, CH2), 3.98-3.83 (m, 1H, CH), 3.58-3.42 (m, 4H, 2 CH2), 2.91 (hept, 1H, J=7.0 Hz, CH), 1.23 (d, 6H, J=7.0 Hz, 2 CH3).

WORKUP

后处理

customThe fumaric acid salt 18 crystallizes from the reaction medium

来源与证据

来源类型: Open Reaction Database
ORD 记录: ord-2338ca1cc3674ef196e45d2d24a3c40a
来源数据集: uspto-grants-2014_04
DOI: 10.6084/m9.figshare.5104873.v1
专利: US08691982B2
来源说明: uspto-grants-2014_04

反应 SMILES

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