HRID2171740

反应详情

EQUATION

反应方程式

HRID 2171740 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a vigorously stirred solution of sodium hydrogen cyanamide (0.52 g, 7.9 mmol) in methanol (20 mL) was added slowly (S)-2-(5,5-dimethyl-5,6,7,8-tetrahydro-naphthalen-2-yloxymethyl)-oxirane (1.8 g, 7.9 mmol). The reaction mixture was stirred at room temperature overnight after which it was concentrated. Anhydrous diethyl ether (100 mL) was added. The resulting white precipitate was filtered and the filtrate concentrated. The residue was purified by flash chromatography (silica, 7N NH3 in methanol/methylene chloride) to give 1.0 g (46%) of 5-(5,5-dimethyl-5,6,7,8-tetrahydro-naphthalen-2-yloxymethyl)-4,5-dihydro-oxazol-2-ylamine.

WORKUP

后处理

  1. concentrationwas concentrated
  2. additionAnhydrous diethyl ether (100 mL) was added
  3. filtrationThe resulting white precipitate was filtered
  4. concentrationthe filtrate concentrated
  5. customThe residue was purified by flash chromatography (silica, 7N NH3 in methanol/methylene chloride)