反応 #1994317

反応方程式

2-(3-chloro-pyridin-2-yl)-5-methoxy-2H-pyrazole-3-carboxylic acid

acetonitrile

6-amino-5-methyl-1H-indazole-7-carboxylic acid

mesylchloride

→

title compound

7-[2-(3-chloro-pyridin-2-yl)-5-methoxy-2H-pyrazol-3-yl]-5-methyl-1H-8-oxa-1,2,6-triaza-benz[e]inden-9-one

溶媒

pyridine

反応条件

後処理

1. 1
   濃縮The reaction mixture was concentrated in vacuo
2. 2
   workup.STIRRINGstirred for 15 min
3. 3
   ろ過The resulting yellow suspension was filtrated
4. 4
   洗浄The filtercake was washed sequentially with water and heptane/AcOEt 2:1
5. 5
   その他dried

実験手順

To a solution of 2-(3-chloro-pyridin-2-yl)-5-methoxy-2H-pyrazole-3-carboxylic acid (40 g, 157 mmol) and acetonitrile (1000 mL) was added 6-amino-5-methyl-1H-indazole-7-carboxylic acid (30 g, 157 mmol). To the resulting brown suspension were added sequentially pyridine (57 mL, 706 mml) and dropwise mesylchloride (43 mL, 549 mmol). The reaction mixture was stirred for 6 h at 50° C. and 15 hours at ambient temperature. The reaction mixture was concentrated in vacuo. The residue was suspended in water and stirred for 15 min. The resulting yellow suspension was filtrated. The filtercake was washed sequentially with water and heptane/AcOEt 2:1 and dried to afford the title compound as beige powder, which was submitted to the next step without further purification. LC/MS: 409 (M+H)+.

出典