HRID592398
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 0 °C
PROCEDURE
实验过程
4-Nitro-1H-pyrazole (0.452 g, 4.00 mmol) was dissolved in DMF (8 mL) and cooled to 0° C. NaH (0.192 g, 60% dispersion in oil, 4.80 mmol) was added and the mixture was stirred for 10 minutes. 1-Methylpyrrolidin-3-yl methanesulfonate A22 (0.717 g, 4.00 mmol) was added and the mixture was stirred for 16 hours at 100° C. The mixture was diluted with EtOAc (5 mL) and washed with sat. NH4Cl (5 mL) and water (4×5 mL). The organics were concentrated in vacuo affording a crude pale yellow oil which was purified by flash chromatography (0-30% MeOH in DCM) to give the title compound A23 as a pale yellow oil (0.575 g, 73% yield). LCMS-B: rt 1.12 min; m/z 197 [M+H]+.
WORKUP
后处理
- addition(0.717 g, 4.00 mmol) was added
- stirringthe mixture was stirred for 16 hours at 100° C
- washwashed with sat. NH4Cl (5 mL) and water (4×5 mL)
- concentrationThe organics were concentrated in vacuo
- customaffording a crude pale yellow oil which
- customwas purified by flash chromatography (0-30% MeOH in DCM)