反应 #2446080

ord-2c48b181bbf344fa9c375c6ba6d9d031

反应方程式

CC(O)CN(C(=O)OC(C)(C)C)C1CCCCC1
tert-butyl cyclohexyl(2-hydroxypropyl)carbamate
Cc1cc(C)c(C(=O)Cl)c(C)c1
2,4,6-trimethyl-benzoyl chloride
Cc1cc(C)c(C(=O)OC(C)CN(C(=O)OC(C)(C)C)C2CCCCC2)c(C)c1
1-((tert-butoxycarbonyl)(cyclohexyl)amino)propan-2-yl 2,4,6-trimethylbenzoate

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他The resultant reaction mixture
  2. 2
    洗涤washed with water and brine
  3. 3
    干燥The organic layer was dried over sodium sulphate
  4. 4
    浓缩concentrated to dryness

实验过程

To a solution of tert-butyl cyclohexyl(2-hydroxypropyl)carbamate (1 g, 3.89 mmol) in dry toluene (10 ml), 2,4,6-trimethyl-benzoyl chloride (0.510 mL, 4.280 mmol) was added. The resultant reaction mixture was stirred at rt for 16 hours. The reaction mixture was diluted in ethyl acetate and washed with water and brine. The organic layer was dried over sodium sulphate, and concentrated to dryness to obtain 1-((tert-butoxycarbonyl)(cyclohexyl)amino)propan-2-yl 2,4,6-trimethylbenzoate. Yield: 1 g (64.10%); LCMS: m/z=404.4 [M+H], RT=2.76 min, (Column: Y, Program: P1)

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US08685418B2uspto-grants-2014_04