反応 #2446080

ord-2c48b181bbf344fa9c375c6ba6d9d031

反応方程式

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

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他The resultant reaction mixture
  2. 2
    洗浄washed with water and brine
  3. 3
    乾燥The organic layer was dried over sodium sulphate
  4. 4
    濃縮concentrated to dryness

実験手順

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)

出典

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