HRID1511063

反应详情

EQUATION

反应方程式

HRID 1511063 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

(R)-2,2,5,5-Tetramethyl-1,3-dioxolane-4-carbaldehyde (16 g, 101 mmol) (Burger, A. Synthesis 1989, (2) 93-97) was dissolved in 1:1 methanol:water (250 mL), and hydroxylamine hydrochloride (7.0 g, 101 mmol) and Na2CO3 (5.4 g, 51 mmol) were added and the reaction was stirred at ambient temperature for 2 hours. The methanol was partially removed in vacuo and the aqueous layer was extracted with CH2Cl2, dried, filtered, and concentrated to afford (S)-2,2,5,5-tetramethyl-1,3-dioxolane-4-carbaldehyde oxime (13 g, 75 mmol, 74% yield) as an amber oil.

WORKUP

后处理

  1. customThe methanol was partially removed in vacuo
  2. extractionthe aqueous layer was extracted with CH2Cl2
  3. customdried
  4. filtrationfiltered
  5. concentrationconcentrated