反応 #1509588

ord-621cc250a12749e2ad2a403d76975118

反応方程式

COC(=O)c1cc(NC(=O)OC(C)(C)C)cc(C(C)(C)C)c1
Methyl 3-(tert.-butoxycarbonylamino)-5-tert-butylbenzoate
O=C(O)C(F)(F)F
TFA
CCOC(=O)c1cc(N)cc(C(C)(C)C)c1
ethyl 3-amino-5-tert-butylbenzoate

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    濃縮concentrated in vacuum
  2. 2
    workup.DISSOLUTIONThe residue was dissolved in DCM
  3. 3
    抽出extracted with aqueous sodium bicarbonate solution
  4. 4
    その他The organic layer was separated
  5. 5
    乾燥dried over sodium sulphate
  6. 6
    濃縮concentrated in vacuum

実験手順

Methyl 3-(tert.-butoxycarbonylamino)-5-tert-butylbenzoate (0.42 g) was dissolved in DCM (5 ml). To the resulting solution, TFA (1 ml) was added, the mixture was stirred for 30 min at room temperature and then concentrated in vacuum. The residue was dissolved in DCM and extracted with aqueous sodium bicarbonate solution. The organic layer was separated, dried over sodium sulphate and concentrated in vacuum to yield ethyl 3-amino-5-tert-butylbenzoate (0.28 g), which was used for the synthesis of example 112 without further purification.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: USRE045323E1uspto-grants-2015_01