HRID1424092

反应详情

EQUATION

反应方程式

REACTANTS

反应物

结构：CSC1=NCCSC(C)(CO[Si](C)(C)C(C)(C)C)C1

HCID68522215

未命名化合物

结构：N#Cc1ccc(-c2ccc(C3(C(=O)NN)CC3)cc2)nc1

HCID86712940

未命名化合物

PRODUCTS

生成物

结构：CC1(CO[Si](C)(C)C(C)(C)C)Cc2nnc(C3(c4ccc(-c5ccc(C#N)cn5)cc4)CC3)n2CCS1

HCID86712941

未命名化合物

收率 89%

AUXILIARIES

试剂、催化剂与溶剂

溶剂HCID263

1-Butanol

C4H10O

PROCEDURE

实验过程

A solution of 7-({[tert-butyl(dimethyl)silyl]oxy}methyl)-7-methyl-5-(methylthio)-2,3,6,7-tetrahydro-1,4-thiazepine (39.7 g, 124 mmol) and the compound (19.5 g, 70.1 mmol) obtained in Example 60-3) in 1-butanol (750 mL) was stirred at 140° C. for 13 h. The reaction mixture was cooled to room temperature, the solvent was distilled off under reduced pressure, and the residue was purified by silica gel column chromatography (ethyl acetate:methanol=9:1) to obtain the title compound (33.1 g, 89%) as a white solid.

WORKUP

后处理

distillationthe solvent was distilled off under reduced pressure
customthe residue was purified by silica gel column chromatography (ethyl acetate:methanol=9:1)

来源与证据

来源类型: Open Reaction Database
ORD 记录: ord-36d73fb6468d46df9274381792ac06d1
来源数据集: uspto-grants-2015_01
DOI: 10.6084/m9.figshare.5104873.v1
专利: US08927536B2
来源说明: uspto-grants-2015_01

反应 SMILES

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