반응 #1509588

ord-621cc250a12749e2ad2a403d76975118

반응 방정식

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

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    농축concentrated in vacuum
  2. 2
    workup.DISSOLUTIONThe residue was dissolved in DCM
  3. 3
    추출extracted with aqueous sodium bicarbonate solution
  4. 4
    기타The organic layer was separated
  5. 5
    건조dried over sodium sulphate
  6. 6
    농축concentrated in vacuum

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: USRE045323E1uspto-grants-2015_01