反应 #587367

ord-04f2c5a25ba54d3190cfc070ca51c1c9

反应方程式

COC(=O)Cl
Methyl chloroformate
NCc1ccc(Br)cc1F
1-(4-bromo-2-fluorophenyl)methanamine
CCN(CC)CC
triethylamine
COC(=O)NCc1ccc(Br)cc1F
methyl (4-bromo-2-fluorobenzyl)carbamate

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他the ice-water bath was removed
  2. 2
    洗涤washed with water, and brine
  3. 3
    干燥The organic layer was dried over Na2SO4
  4. 4
    过滤filtered
  5. 5
    浓缩concentrated under reduced pressure
  6. 6
    其他The residue (220 mg, 83.9%) was directly used in next step without further purification

实验过程

Methyl chloroformate (85.0 μL, 1.1 mmol) was added to a solution of 1-(4-bromo-2-fluorophenyl)methanamine (0.204 g, 1.0 mmol) and triethylamine (148.1 μL, 1.1 mmol) in methylene chloride (5 mL) at 0° C. After 10 min, the ice-water bath was removed. The mixture was stirred at RT for 1 h, washed with water, and brine. The organic layer was dried over Na2SO4, filtered, and concentrated under reduced pressure. The residue (220 mg, 83.9%) was directly used in next step without further purification. LCMS: (M+H)=263.9/261.8.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07767675B2uspto-grants-2010_08