반응 #51431

ord-cdd6a8e0b30745f3a6723f492fb8731a

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.ADDITIONwas added
  2. 2
    세척The flask was rinsed 3 times with hydrogen
  3. 3
    workup.ADDITIONfilled with hydrogen at 30 to 35 psi
  4. 4
    여과The catalyst was filtered off
  5. 5
    기타the filtrate was evaporated in vacuo to dryness

실험 절차

To a solution of 6-Nitro-1H-indole-2-carboxylic acid methyl ester (108) 200 mg (0.91 mmole) in a mixture of methanol/ethylacetate 1:1 10% Pd/C (40 mg) was added. The flask was rinsed 3 times with hydrogen and filled with hydrogen at 30 to 35 psi. The suspension was stirred vigorously at room temperature for 30 minutes. The catalyst was filtered off, the filtrate was evaporated in vacuo to dryness. The resulted 6-amino-1H-indole-2-carboxylic acid methyl ester gave a single spot on TLC (Silica, toluene-ethylacetate 7:3, Rf:0.31) and was used for the next step without purification

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US06849713B2uspto-grants-2005_02