HRID624246

反应详情

EQUATION

反应方程式

HRID 624246 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
-15 °C

PROCEDURE

实验过程

HCl (1.55 g, 8.03 mmol) was suspended in dimethylformamide (30 ml) and treated with triisopropylethylamine (4.21 ml, 24.08 mmol). After stirring for 20 minutes, the mixture was cooled to −15° C. 2-(4-Isocyanatophenyl)-4,4,5,5-tetramethyl-1,3,2-dioxaborolane (2.028 g, 8.03 mmol) was dissolved in 10 ml tetrahydrofuran and added via syringe over 10 minutes. The mixture was allowed to warm to room temperature, and it was stirred for 3 hours and concentrated under a stream of nitrogen to minimal volume. The residue was diluted with cold water to give a turbid mixture which was filtered with water washes to provide the title compound after drying.

WORKUP

后处理

  1. additionadded via syringe over 10 minutes
  2. temperatureto warm to room temperature
  3. stirringit was stirred for 3 hours
  4. concentrationconcentrated under a stream of nitrogen to minimal volume
  5. additionThe residue was diluted with cold water
  6. customto give a turbid mixture which
  7. filtrationwas filtered with water