反応 #171976

反応方程式

tert-butyl (1S,2R)-2-(4-cyano-3-(1-methyl-1H-indol-4-ylamino)phenylamino)cyclohexylcarbamate

K2CO3

H2O2

Water

→

titled compound

収率 13.9%

4-((1R,2S)-2-aminocyclohexylamino)-2-(1-methyl-1H-indol-4-ylamino)benzamide

収率 13.9%

溶媒

EtOAc

DMSO

反応条件

後処理

1. 1
   その他The organic phase was separated
2. 2
   乾燥dried over Na2SO4
3. 3
   濃縮concentrated in vacuo
4. 4
   workup.DISSOLUTIONThe residue was dissolved in TFA (2 mL)
5. 5
   workup.WAITAfter 10 min of standing
6. 6
   その他TFA was removed in vacuo
7. 7
   その他The residue was purified by HPLC

実験手順

To a solution of tert-butyl (1S,2R)-2-(4-cyano-3-(1-methyl-1H-indol-4-ylamino)phenylamino)cyclohexylcarbamate (90 mg, 0.19 mmol) in DMSO (2 mL). K2CO3 (130 mg, 0.94 mmol) and H2O2 (50% aq., 0.500 mL) were added. The mixture was stirred at 100 C for 10 min. Water and EtOAc were added. The organic phase was separated, dried over Na2SO4, concentrated in vacuo. The residue was dissolved in TFA (2 mL). After 10 min of standing, TFA was removed in vacuo. The residue was purified by HPLC to give the titled compound (10 mg). MS 378.3 (M+H); UV 224.7, 291.5 nm

出典