HRID70053

反应详情

EQUATION

反应方程式

HRID 70053 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The guanidine (b) was dissolved in HCl (5 mL, 6 M) at 0° C. and then stirred for 2 h. After the starting material was consumed, NaOH (25%) was added until a precipitate formed. This mixture was stirred for 30 min. The reaction was then poured into NaOH (0.5 M), extracted with CH2Cl2, dried and concentrated. Flash chromatography afforded (c) (0.95 g, 50%). NMR (500 MHz, DMSO-d6) δ 8.58 (s, br, 1H), 7.34-6.74 (m, 5H), 6.68 (s, 2H), 6.62 (br, 2H), 3.82 (s, 6H), 3.73 (s, 3H). MS: 157.6 (M−H)−; 160.0 (M+H)+.

WORKUP

后处理

  1. customAfter the starting material was consumed
  2. additionNaOH (25%) was added until a precipitate
  3. customformed
  4. stirringThis mixture was stirred for 30 min
  5. extractionextracted with CH2Cl2
  6. customdried
  7. concentrationconcentrated