HRID1369354

反应详情

EQUATION

反应方程式

HRID 1369354 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The procedure of Example 1 is repeated using 1.95 g (12.5 mmol) of 1-oxyl-2,2,6,6-tetramethylpiperidine, 6.19 g (60 mmol) of tert-butyl nitrite, 7.6 mg (0.0125 mmol) of (S,S)-(+)-N,N-bis(3,5-di-tert-butylsalicylidene)-1,2-cyclohexanediaminocobalt(II), 80 mL of pyridine and 5.30 g (25 mmol) of 4,4′-diaminobenzophenone at 70° C. The crude product obtained is purified by vacuum flash chromatography (1% ethyl acetate in heptane) to give 0.6 g of the title compound as a yellow solid in 9.17% yield. The structure is confirmed by 1Hnmr and mass spectrographic analysis.

WORKUP

后处理

  1. customat 70° C
  2. customThe crude product obtained
  3. customis purified by vacuum flash chromatography (1% ethyl acetate in heptane)