HRID1811571

反应详情

EQUATION

反应方程式

HRID 1811571 的结构方程式

PROCEDURE

实验过程

To an ice-cooled solution of 6-chloro-2-methyl-3-nitropyridine (2.17 g, 13 mmol) in 2-mercaptoethanol (5 mL, 71 mmol), potassium hydroxide (1.52 g, 27 mmol) was added. Mixture was stirred at room temperature for 2 h and then extracted with NaOH solution and CH2Cl2. Organic phases were dried over MgSO4, filtered, and concentrated to give 2-(6-methyl-5-nitro-pyridin-2-ylsulfanyl)-ethanol as a brown oil (60% pure, 3.25 g, 72%). 1HNMR (CDCl3, 400 MHz) δ 2.87-2.90 (m, 6H), 3.43-3.46 (t, J=5.6 Hz, 2H), 7.22-7.24 (d, J=8.7 Hz, 1H), 8.15-8.17 (d, J=8.7 Hz, 1H). Exact mass calculated for C8H10N2O3S 214.04 found 215.1 (MH+).

WORKUP

后处理

  1. additionwas added
  2. extractionextracted with NaOH solution and CH2Cl2
  3. dry with materialOrganic phases were dried over MgSO4
  4. filtrationfiltered
  5. concentrationconcentrated