反応 #2069939

ord-4703ea5ae80e44aaafd8da2ad06efb87

反応方程式

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
収率 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
収率 101.6%

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他evaporated to dryness
  2. 2
    workup.DISSOLUTIONThe resulting residue was dissolved in DCM
  3. 3
    洗浄the solution was washed with brine
  4. 4
    workup.ADDITIONtreated with NaHCO3 aq. The obtained precipitate
  5. 5
    ろ過was filtered
  6. 6
    洗浄washed with water and DCM
  7. 7
    その他dried under vacuum

実験手順

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.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07541354B2uspto-grants-2009_06