HRID456948

反应详情

EQUATION

反应方程式

HRID 456948 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of the product of Example 9 (175 mg), dimethylamine hydrochloride (64 mg), and acetic acid (0.05 mL) in DCE (3 mL) was treated with sodium triacetoxyborohydride (210 mg). After 16 h, the resulting mixture was treated with 10% sodium hydroxide (1 mL) and extracted with DCM (3×3 mL). The combined organic phases were dried (magnesium sulfate) and evaporated. Chromatography of the residue (3% 2 M methanolic ammonia/DCM) gave the title compound as a colorless oil (70 mg). 1H NMR (400 MHz, CDCl3): 7.19 (d, J=8.6 Hz, 2H), 6.85 (d, J=8.6 Hz, 2H), 3.99 (t, J=6.4 Hz, 2H), 3.35 (s, 2H), 2.50–2.35 (m, 6H), 2.22 (s, 6H), 2.01–1.94 (m, 2H), 1.63–1.55 (m, 4H), 1.46–1.40 (m, 2H).

WORKUP

后处理

  1. extractionextracted with DCM (3×3 mL)
  2. dry with materialThe combined organic phases were dried (magnesium sulfate)
  3. customevaporated