HRID2424793

反应详情

EQUATION

反应方程式

HRID 2424793 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

6-[(3S,4S)-1-benzyl-4-methylpyrrolidin-3-yl]-1-(tetrahydro-2H-pyran-4-yl)-1,5-dihydro-4H-pyrazolo[3,4-d]pyrimidin-4-one (5.6 g) was dissolved in 100 mL of methanol and added to a Parr bottle. Palladium hydroxide (3.76 g) was added along with 3.56 mL of concentrated hydrochloric acid. The reaction mixture was placed on a hydrogenator under 40 psi of H2 for 18 h. The reaction mixture was filtered through Celite and concentrated to provide 4.47 g of the title compound as the hydrogen chloride salt. 400 MHz 1H NMR (CD3OD) δ 8.03 (s, 1H), 4.49 (m, 1H), 4.09-4.06 (m, 2H), 3.74-3.57 (m, 4H), 3.24 (m, 1H), 3.05 (m, 1H), 2.89 (m, 1H), 2.77 (m, 1H), 2.30 (m, 2H), 1.90 (m, 2H), 1.22 (d, J=6.6 Hz, 3H). MS: (M+H m/z=304.2).

WORKUP

后处理

  1. additionadded to a Parr bottle
  2. filtrationThe reaction mixture was filtered through Celite
  3. concentrationconcentrated