反应 #1509588

ord-621cc250a12749e2ad2a403d76975118

反应方程式

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

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    浓缩concentrated in vacuum
  2. 2
    workup.DISSOLUTIONThe residue was dissolved in DCM
  3. 3
    萃取extracted with aqueous sodium bicarbonate solution
  4. 4
    其他The organic layer was separated
  5. 5
    干燥dried over sodium sulphate
  6. 6
    浓缩concentrated in vacuum

实验过程

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.

来源

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