HRID927016

反应详情

EQUATION

反应方程式

REACTANTS

反应物

结构：CC[N+](CC)(CC)S(=O)(=O)NC(=O)OC.[OH-]

HCID11032497

(Methoxycarbonylsulfamoyl)triethylammonium hydroxide

C8H20N2O5S

结构：CC(=O)C1=C(C)N(c2cccc(C(F)(F)F)c2)C(=O)N(C)C1c1ccc(C#N)cc1C(=O)N(N)C(C)=O

HCID118691673

未命名化合物

2 次

PRODUCTS

生成物

结构：CC(=O)C1=C(C)N(c2cccc(C(F)(F)F)c2)C(=O)N(C)C1c1ccc(C#N)cc1-c1nnc(C)o1

HCID118691694

未命名化合物

AUXILIARIES

试剂、催化剂与溶剂

溶剂HCID6344

Dichloromethane

CH2Cl2

PROCEDURE

实验过程

2-[5-Acetyl-3,6-dimethyl-2-oxo-1-(3-trifluoromethyl-phenyl)-1,2,3,4-tetrahydro-pyrimidin-4-yl]-5-cyano-benzoic acid acetyl hydrazide (intermediate 13) (15 mg, 0.03 mmol) is suspended in dichloromethane (1 mL) and (methoxycarbonylsulfamoyl)triethyl-ammonium hydroxide (Burgess reagent)(17.4 mg, 0.07 mmol) is added. The mixture is stirred at room temperature for 3 days. The solvent is removed under reduced pressure and purification is performed by reversed phase HPLC. Yield: 6.4 mg; ESI mass spectrum [M+H]+=496; Retention time HPLC: 1.04 min (HPLC method Z018_S04).

WORKUP

后处理

customThe solvent is removed under reduced pressure and purification
custom1.04 min (HPLC method Z018_S04)

来源与证据

来源类型: Open Reaction Database
ORD 记录: ord-7654b0ec4a364ab8ad060ed56a5b15cb
来源数据集: uspto-grants-2016_03
DOI: 10.6084/m9.figshare.5104873.v1
专利: US09290457B2
来源说明: uspto-grants-2016_03

反应 SMILES

C([N:4]([C:6](=[O:37])[C:7]1[CH:12]=[C:11]([C:13]#[N:14])[CH:10]=[CH:9][C:8]=1[CH:15]1[C:20]([C:21](=O)[CH3:22])=[C:19]([CH3:24])[N:18]([C:25]2[CH:30]=[CH:29][CH:28]=[C:27]([C:31]([F:34])([F:33])[F:32])[CH:26]=2)[C:17](=[O:35])[N:16]1[CH3:36])[NH2:5])(=O)C.[OH-:38].COC(NS([N+](CC)(CC)[CH2:48][CH3:49])(=O)=O)=O>ClCCl>[C:21]([C:20]1[CH:15]([C:8]2[CH:9]=[CH:10][C:11]([C:13]#[N:14])=[CH:12][C:7]=2[C:6]2[O:37][C:48]([CH3:49])=[N:5][N:4]=2)[N:16]([CH3:36])[C:17](=[O:35])[N:18]([C:25]2[CH:30]=[CH:29][CH:28]=[C:27]([C:31]([F:33])([F:34])[F:32])[CH:26]=2)[C:19]=1[CH3:24])(=[O:38])[CH3:22]