HRID1789545

反应详情

EQUATION

反应方程式

HRID 1789545 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3-(5-[(1,1-Dimethylethyl)dimethylsiloxy]pent-1-yl)cyclopentene (300 g, 1.170 moles) is diluted with acetonitrile (3000 ml) and a 40% stock solution of hydrofluoric acid (166 ml) is added. The reaction is stirred at room temperature for 10 minutes and then slowly neutralized with a saturated solution of sodium bicarbonate. The reaction is partitioned between ether (1500 ml) and the aqueous phase extracted with ether (1×1000 ml). The organic layers are combined and the solvent volume is reduced under vacuum. The residue is dried over anhydrous sodium sulfate and the remaining solvent removed leaving a clear, colorless oil. The product is kugelrohred under vacuum leaving a product sufficiently pure for the next reaction (171 g, 1.11 moles).

WORKUP

后处理

  1. customThe reaction is partitioned between ether (1500 ml)
  2. extractionthe aqueous phase extracted with ether (1×1000 ml)
  3. dry with materialThe residue is dried over anhydrous sodium sulfate
  4. customthe remaining solvent removed
  5. customleaving a clear, colorless oil
  6. customleaving a product
  7. customsufficiently pure for the next reaction (171 g, 1.11 moles)