HRID271347

反应详情

EQUATION

反应方程式

HRID 271347 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 2 g of 3-tert-butoxycarbonylmethylene-cyclobutanecarboxylic acid, 150 mL of ethanol, 0.5 g of 5% platinum on carbon, and 200 mL of ethanol was stirred under 1 atm of hydrogen for 48 h overnight, filtered, diluted with 20 mL of toluene and concentrated under reduced pressure. Drying under vacuum overnight gave 2 g of product, which was predominantly as a colorless oil: 1H NMR (400 MHz, CDCl3) 10.2 (br s, 1H), 3.0 (m, 1H), 2.3 (m, 1H), 2.38 (m, 4H), 2.0 (dd, 2H), 1.4 (s, 9).

WORKUP

后处理

  1. filtrationfiltered
  2. additiondiluted with 20 mL of toluene
  3. concentrationconcentrated under reduced pressure
  4. customDrying under vacuum overnight