HRID1519527

反应详情

EQUATION

反应方程式

HRID 1519527 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To the di-tert-butyl(4-cyano-2,5-difluorophenyl)propanedioate (10.0 g, 28.3 mmol) in dichloromethane (30 mL) was added triflouroacetic acid (10 mL) and the mixture stirred for 12 h at room temperature. The solution was concentrated under reduced pressure and chased with toluene (2×) to give the crude product as a yellowish oil (5 g, 90%, 85% purity as indicated by NMR). The residue was used in the next step without further purification. 1H NMR (500 MHz, CDCl3) δ 7.31 (dd, J=3, J=2 Hz, 1H), 7.21 (dd, J=5.8, J=5.8 Hz, 1H), 3.67 (s, 2H). LC-MS (IE, m/z): 198 [M+1]+.

WORKUP

后处理

  1. concentrationThe solution was concentrated under reduced pressure and chased with toluene (2×)