반응 #2069939

ord-4703ea5ae80e44aaafd8da2ad06efb87

반응 방정식

CCOC(=O)n1nc(NC(=O)C(C)c2ccc3ccccc3c2)c2c1CN(C(=O)OC(C)(C)C)C2
3-(2-naphthalen-2-yl-propionylamino)-4,6-dihydro-pyrrolo[3,4-c]pyrazole-1,5-dicarboxylic acid 5-tert-butyl ester 1-ethyl ester
ClCCl.O=C(O)C(F)(F)F
TFA DCM
CCOC(=O)n1nc(NC(=O)C(C)c2ccc3ccccc3c2)c2c1CNC2
title compound
수율 101.6%
CCOC(=O)n1nc(NC(=O)C(C)c2ccc3ccccc3c2)c2c1CNC2
3-(2-Naphthalen-2-yl-propionylamino)-5,6-dihydro-4H-pyrrolo[3,4-c]pyrazole-1-carboxylic acid ethyl ester
수율 101.6%

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타evaporated to dryness
  2. 2
    workup.DISSOLUTIONThe resulting residue was dissolved in DCM
  3. 3
    세척the solution was washed with brine
  4. 4
    workup.ADDITIONtreated with NaHCO3 aq. The obtained precipitate
  5. 5
    여과was filtered
  6. 6
    세척washed with water and DCM
  7. 7
    기타dried under vacuum

실험 절차

2.5 g (5.2 mmol) of 3-(2-naphthalen-2-yl-propionylamino)-4,6-dihydro-pyrrolo[3,4-c]pyrazole-1,5-dicarboxylic acid 5-tert-butyl ester 1-ethyl ester in 15 ml DCM was treated with 16 ml of (1:1) TFA/DCM. The reaction mixture was stirred for 30 min. and evaporated to dryness. The resulting residue was dissolved in DCM and the solution was washed with brine and then treated with NaHCO3 aq. The obtained precipitate was filtered, washed with water and DCM, and then dried under vacuum to give 2.0 g (quantitative yield) of the title compound.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07541354B2uspto-grants-2009_06