氯甲酸甲酯 → Methyl (4-bromo-2-fluorobenzyl)carbamate

HRID 500185

反应方程式

HRID 500185 反应方程式
Cl[C:2]([O:4][CH3:5])=[O:3].[Br:6][C:7]1[CH:12]=[CH:11][C:10]([CH2:13][NH2:14])=[C:9]([F:15])[CH:8]=1.C(N(CC)CC)C>C(Cl)Cl>[Br:6][C:7]1[CH:12]=[CH:11][C:10]([CH2:13][NH:14][C:2](=[O:3])[O:4][CH3:5])=[C:9]([F:15])[CH:8]=1

参与物

5

反应物 3

HCID 6586氯甲酸甲酯HCID 8471三乙胺HCID 37708484-溴-2-氟苄胺

产物 1

HCID 19695032Methyl (4-bromo-2-fluorobenzyl)carbamate

试剂、催化剂与溶剂 1

HCID 6344二氯甲烷溶剂

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.

后处理

  1. customthe ice-water bath was removed
  2. washwashed with water, and brine
  3. dry with materialThe organic layer was dried over Na2SO4
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure
  6. customThe residue (220 mg, 83.9%) was directly used in next step without further purification

来源与证据

ORD记录
ord-04f2c5a25ba54d3190cfc070ca51c1c9
来源数据集
uspto-grants-2010_08
专利号
US07767675B2

关联笔记

加载中…