HRID1619590

反应详情

EQUATION

反应方程式

REACTANTS

反应物

结构：COc1ccc(CN(c2ncns2)S(=O)(=O)c2ccc(Oc3ccc(-c4ccc(C(F)(F)F)cc4)cc3-c3ccnnc3)c(C#N)c2)c(OC)c1

HCID58042256

未命名化合物

PRODUCTS

生成物

结构：N#Cc1cc(S(=O)(=O)Nc2ncns2)ccc1Oc1ccc(-c2ccc(C(F)(F)F)cc2)cc1-c1ccnnc1

HCID56600788

未命名化合物

收率 45.7%

AUXILIARIES

试剂、催化剂与溶剂

溶剂HCID313

Hydrochloric Acid

ClH

溶剂HCID31275

1,4-Dioxane

C4H8O2

PROCEDURE

实验过程

3-Cyano-N-(2,4-dimethoxybenzyl)-4-{[3-pyridazin-4-yl-4′-(trifluoromethyl)biphenyl-4-yl]oxy}-N-1,2,4-thiadiazol-5-ylbenzenesulfonamide (Preparation 26, 210 mg, 0.29 mmol) was dissolved a in 4M solution of hydrogen chloride in 1,4-dioxane (7 mL) and stirred at room temperature for 5 hours. A precipitate formed which was collected by filtration and purified by trituration with dichloromethane followed by silica gel column chromatography (0%-15% methanol in dichloromethane gradient elution) to afford the title compound as a solid (77 mg, yield).

WORKUP

后处理

customA precipitate formed which
filtrationwas collected by filtration
custompurified by trituration with dichloromethane
washfollowed by silica gel column chromatography (0%-15% methanol in dichloromethane gradient elution)

来源与证据

来源类型: Open Reaction Database
ORD 记录: ord-36a80d27fa5744f9a72598b6229e705a
来源数据集: uspto-grants-2014_07
DOI: 10.6084/m9.figshare.5104873.v1
专利: US08772293B2
来源说明: uspto-grants-2014_07

反应 SMILES

[C:1]([C:3]1[CH:4]=[C:5]([S:32]([N:35](CC2C=CC(OC)=CC=2OC)[C:36]2[S:40][N:39]=[CH:38][N:37]=2)(=[O:34])=[O:33])[CH:6]=[CH:7][C:8]=1[O:9][C:10]1[CH:15]=[CH:14][C:13]([C:16]2[CH:21]=[CH:20][C:19]([C:22]([F:25])([F:24])[F:23])=[CH:18][CH:17]=2)=[CH:12][C:11]=1[C:26]1[CH:31]=[CH:30][N:29]=[N:28][CH:27]=1)#[N:2]>Cl.O1CCOCC1>[C:1]([C:3]1[CH:4]=[C:5]([S:32]([NH:35][C:36]2[S:40][N:39]=[CH:38][N:37]=2)(=[O:33])=[O:34])[CH:6]=[CH:7][C:8]=1[O:9][C:10]1[CH:15]=[CH:14][C:13]([C:16]2[CH:17]=[CH:18][C:19]([C:22]([F:25])([F:23])[F:24])=[CH:20][CH:21]=2)=[CH:12][C:11]=1[C:26]1[CH:31]=[CH:30][N:29]=[N:28][CH:27]=1)#[N:2]