反応 #595382

反応方程式

methyl 3-amino-4-methylbenzoate

sodium nitrite

→

title compound

methyl 1H-indazole-6-carboxylate

溶媒

AcOH

H2O

反応条件

後処理

1. 1
   workup.ADDITIONAfter addition
2. 2
   その他Then half of the solvent was removed under reduced pressure
3. 3
   workup.ADDITIONthe resulting mixture was diluted with H2O
4. 4
   抽出extracted with EtOAc
5. 5
   洗浄The combined organics were washed H2O and brine
6. 6
   濃縮concentrated

実験手順

To a solution of methyl 3-amino-4-methylbenzoate D-1 (5.0 g, 30 mmol) in AcOH (140 mL) at 0° C. was added a solution of sodium nitrite (2.1 g, 30 mmol) in H2O (3.5 mL). After addition, the mixture was stirred at rt for 24 h. Then half of the solvent was removed under reduced pressure and the resulting mixture was diluted with H2O, and extracted with EtOAc. The combined organics were washed H2O and brine, and concentrated to give the title compound. LCMS (ESI) calc'd for C9H9N2O2 [M+H]+: 177. found 177.

出典