HRID2390421

反应详情

EQUATION

反应方程式

HRID 2390421 的结构方程式

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

To a mixture of Example 168C (0.10 g, 0.325 mmol) in 2 mL of water was added 1.5 mL 6 M HCl. The resulting solution was cooled to 0° C. and NaNO2 (0.034 g, 0.488 mmol), dissolved in 1 mL water, was added dropwise. The resulting mixture was stirred for 30 minutes at 0° C. and subsequently heated to 90° C. for one hour. After cooling, contents were filtered and the precipitate was washed with 10 mL water and dried under reduced pressure to provide the product in 47% yield as a brown solid in HCl salt form, which was used without further purification. 1H NMR (CD3OD, 300 MHz) δ 8.10 (d, J=9 Hz, 1H), 7.82 (d, J=3 Hz, 1H), 7.60 (dd, J=3, 9 Hz, 1H), 3.89-3.76 (m, 2H), 3.58-3.53 (m, 1H) 3.42-3.23 (m, 4H), 2.38-2.30 (m, 1H), 2.16-2.06 (m, 2H), 1.83-1.75 (m, 1H), 1.51 (d, J=6 Hz, 3H). MS (ESI) [M]+ at 336.

WORKUP

后处理

  1. additionwas added dropwise
  2. temperaturesubsequently heated to 90° C. for one hour
  3. temperatureAfter cooling
  4. filtrationcontents were filtered
  5. washthe precipitate was washed with 10 mL water
  6. customdried under reduced pressure
  7. customto provide the product in 47% yield as a brown solid in HCl salt form, which
  8. customwas used without further purification