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HRID469654

反应详情

EQUATION

反应方程式

HRID 469654 的结构方程式

REACTANTS

反应物

3
结构：CCN(CC)CC
HCID8471

Triethylamine

C6H15N

结构：C#Cc1ccccc1
HCID10821

Phenylacetylene

C8H6

结构：O=c1[nH]nc(Cl)c2ccccc12
HCID2775142

4-chlorophthalazin-1(2H)-one

C8H5ClN2O

PRODUCTS

生成物

1
结构：O=c1[nH]nc(C#Cc2ccccc2)c2ccccc12
HCID67160047

未命名化合物

AUXILIARIES

试剂、催化剂与溶剂

4
结构：[Cu][I]
催化剂HCID24350

Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI)

CuI

结构：c1ccc([P](c2ccccc2)(c2ccccc2)[Pd]([P](c2ccccc2)(c2ccccc2)c2ccccc2)([P](c2ccccc2)(c2ccccc2)c2ccccc2)[P](c2ccccc2)(c2ccccc2)c2ccccc2)cc1
催化剂HCID178418397

未命名化合物

结构：CN(C)C=O
溶剂HCID6228

N,N-Dimethylformamide

C3H7NO

结构：CCOC(C)=O
溶剂HCID8857

Ethyl acetate

C4H8O2

PROCEDURE

实验过程

A mixture of 4-chlorophthalazin-1(2H)-one, ethynylbenzene, triethylamine, copper(I) iodide, and Pd(PPh3)4 in DMF was microwaved at 185° C. for 30 minutes, diluted with EtOAc, washed with water and saturated aqueous NH4Cl, and chromatographed to give impure 4-(phenylethynyl)phthalazin-1(2H)-one, which was used without further purification. This material was treated with O-(diphenylphosphoryl)hydroxylamine as in Example 1B to give impure 2-amino-4-(phenylethynyl)phthalazin-1(2H)-one.

WORKUP

后处理

  1. customwas microwaved at 185° C. for 30 minutes
  2. washwashed with water and saturated aqueous NH4Cl
  3. customchromatographed