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HRID517231

反应详情

EQUATION

反应方程式

HRID 517231 的结构方程式

REACTANTS

反应物

3
结构：O
HCID962

Water

H2O

结构：CN(C)C=O
HCID6228

N,N-Dimethylformamide

C3H7NO

结构：CC1(C)CCC2=C(C1=O)C(c1ccc(Br)cc1)NC(=O)N2c1cccc(C(F)(F)F)c1
HCID86732297

未命名化合物

2 次

PRODUCTS

生成物

1
结构：CC1(C)CCC2=C(C1=O)C(c1ccc(C#N)cc1)NC(=O)N2c1cccc(C(F)(F)F)c1
HCID86732351

未命名化合物

AUXILIARIES

试剂、催化剂与溶剂

1
结构：[C-]#N.[C-]#N.[Zn+2]
催化剂HCID11186

Zinc cyanide (Zn(CN)2)

C2N2Zn

CONDITIONS

反应条件

温度
110 °C

PROCEDURE

实验过程

Under an atmosphere of argon, a mixture of 4-(4-bromophenyl)-6,6-dimethyl-1-(3-(tri-fluoromethyl)phenyl)-3,4,7,8-tetrahydroquinazoline-2,5(1H,6H)-dione (intermediate 7, 372 mg, 0.754 mmol), zinc cyanide (110 mg, 0.937 mmol) and tetrakis(triphenyl-phosphine)palladium(O) (50 mg, 43 μmol) in N,N-dimethylformamide (2 mL) is heated at 110° C. over night. Water is added and the mixture is filtered. The precipitate is purified by flash chromatography on silica (gradient cyclohexane/ethyl acetate 80:20 to 60:40). Yield: 220 mg; ESI mass spectrum [M+H]+=440; Retention time HPLC: 1.26 min (Z005—001).

WORKUP

后处理

  1. filtrationthe mixture is filtered
  2. customThe precipitate is purified by flash chromatography on silica (gradient cyclohexane/ethyl acetate 80:20 to 60:40)
  3. custom1.26 min (Z005—001)