HRID592398

反应详情

EQUATION

反应方程式

HRID 592398 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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

  1. addition(0.717 g, 4.00 mmol) was added
  2. stirringthe mixture was stirred for 16 hours at 100° C
  3. washwashed with sat. NH4Cl (5 mL) and water (4×5 mL)
  4. concentrationThe organics were concentrated in vacuo
  5. customaffording a crude pale yellow oil which
  6. customwas purified by flash chromatography (0-30% MeOH in DCM)