反応 #1617

反応方程式

Lithium aluminium hydride

5-Benzyloxy-2-hydroxy benzoic acid methyl ester

→

4-benzyloxy-2-hydroxymethyl phenol

溶媒

tetrahydrofuran

tetrahydrofuran

反応条件

後処理

1. 1
   温度The mixture was warmed to room temperature
2. 2
   温度The reaction was then cooled to 0° C.
3. 3
   その他cautiously quenched by the addition of water (0.5 ml), 2M sodium hydroxide solution (0.5 ml), and water (1 ml)
4. 4
   workup.STIRRINGThe resulting mixture was stirred at room temperature for 30 minutes
5. 5
   ろ過filtered
6. 6
   その他The filtrate was evaporated in vacuo

実験手順

Lithium aluminium hydride (0.235 g, 6.2 mMol) was suspended in tetrahydrofuran (25 ml) and cooled to 0° C. 5-Benzyloxy-2-hydroxy benzoic acid methyl ester (2 g, 7.75 mMol) in tetrahydrofuran (10 ml) was added dropwise, via cannula. The mixture was warmed to room temperature and stirred for 20 minutes. The reaction was then cooled to 0° C. and cautiously quenched by the addition of water (0.5 ml), 2M sodium hydroxide solution (0.5 ml), and water (1 ml). The resulting mixture was stirred at room temperature for 30 minutes and filtered. The filtrate was evaporated in vacuo to yield 4-benzyloxy-2-hydroxymethyl phenol as a clear oil which was used in the next step without further purification.

出典