HRID63835

反应详情

EQUATION

反应方程式

HRID 63835 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

Into a 250-mL round-bottom flask, was placed N-(3-chloropropyl)-2,2,2-trifluoroacetamide (6 g, 31.65 mmol, 1.00 equiv), tetrahydrofuran (30 mL), BH3/THF (80 mL). The resulting solution was stirred for 3 h at 80° C. in an oil bath. The resulting mixture was concentrated under vacuum. The resulting solution was diluted with 200 mL of H2O. The resulting solution was extracted with 4×100 mL of ethyl acetate and the organic layers combined. The resulting mixture was washed with 2×100 mL of brine. The mixture was dried over anhydrous sodium sulfate. This resulted in 5 g (90%) of (3-chloropropyl)(2,2,2-trifluoroethyl)amine as a light yellow liquid.

WORKUP

后处理

  1. customInto a 250-mL round-bottom flask, was placed
  2. concentrationThe resulting mixture was concentrated under vacuum
  3. additionThe resulting solution was diluted with 200 mL of H2O
  4. extractionThe resulting solution was extracted with 4×100 mL of ethyl acetate
  5. washThe resulting mixture was washed with 2×100 mL of brine
  6. dry with materialThe mixture was dried over anhydrous sodium sulfate
  7. customThis resulted in 5 g (90%) of (3-chloropropyl)(2,2,2-trifluoroethyl)amine as a light yellow liquid