反応 #540783

反応方程式

Indium

2,2-dimethoxyacetaldehyde

allyl bromide

→

product

収率 53.1%

2-hydroxy-1,1-dimethoxy-pent-4-ene

収率 53.1%

溶媒

ethanol

反応条件

後処理

1. 1
   その他the supernatant was decanted
2. 2
   洗浄washed 3 times with ethanol (350, 350, and 450 mL)
3. 3
   workup.ADDITIONThe combined supernatants were mixed with 1500 mL
4. 4
   抽出The crude product was extracted with chloroform (1500, 300 mL)
5. 5
   洗浄The combined organic layers were washed with 1500 mL saturated sodium chloride
6. 6
   抽出The chloroform extract
7. 7
   乾燥was dried over sodium sulfate
8. 8
   ろ過filtered
9. 9
   その他evaporated at reduced pressure

実験手順

Indium powder (0.52 mol, 1 eq., 60 g, 100 mesh) was added to an ethanol (250 mL) solution containing 2,2-dimethoxyacetaldehyde (0.52 mol, 1.0 eq., 90.62 g, 60 wt % solution in water) and allyl bromide (0.79 mol, 1.5 eq., 66.5 mL). The suspension was stirred at 40° C. for 3 h. The slurry was then centrifuged and the supernatant was decanted. The pellet was suspended and washed 3 times with ethanol (350, 350, and 450 mL). The combined supernatants were mixed with 1500 mL deionized water and 1500 mL saturated sodium chloride. The crude product was extracted with chloroform (1500, 300 mL). The combined organic layers were washed with 1500 mL saturated sodium chloride. The chloroform extract was dried over sodium sulfate, filtered and evaporated at reduced pressure. Yield 40.4 g (53% yield) product.

出典