反应 #1502

ord-169f88b27a294c15b3d94e8de0e682c6

反应方程式

O=C(Cl)OCCl
Chloromethyl chloroformate
CC(C)CCC[C@@H](C)[C@H]1CC[C@H]2[C@@H]3CC=C4C[C@@H](O)CC[C@]4(C)[C@H]3CC[C@]12C
cholesterol
c1ccncc1
Pyridine
CC(C)CCC[C@@H](C)[C@H]1CC[C@H]2[C@@H]3CC=C4C[C@](O)(C(=O)OCCl)CC[C@]4(C)[C@H]3CC[C@]12C
3-(Chloromethoxycarbonyl) Cholesterol

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度The solution was cooled
  2. 2
    温度Heat
  3. 3
    其他was produced
  4. 4
    其他the reaction gave a clear solution from
  5. 5
    洗涤washed with 0.5M HCl (50 ml) and water (3×25 ml)
  6. 6
    其他After treatment with MgSO4, the solution was evaporated to dryness

实验过程

Chloromethyl chloroformate (1.96 g, 15.2 mmol) and cholesterol (5.0 g, 12.9 mmol) was dissolved in CH2Cl2 (10 ml). The solution was cooled. Pyridine (1.21 g, 15.3 mmol) was dripped into the stirred solution over 5 minutes. Heat was produced and the reaction gave a clear solution from a somewhat unclear starting solution. After 24 hours at room temperature, the mixture was diluted with CH2Cl2 (50 ml), washed with 0.5M HCl (50 ml) and water (3×25 ml). After treatment with MgSO4, the solution was evaporated to dryness.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US05725840uspto-grants-1998_03