Allyl bromide → HCID 10329416, compound

Temperature

40 °C

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.

1. customthe supernatant was decanted
2. washwashed 3 times with ethanol (350, 350, and 450 mL)
3. additionThe combined supernatants were mixed with 1500 mL
4. extractionThe crude product was extracted with chloroform (1500, 300 mL)
5. washThe combined organic layers were washed with 1500 mL saturated sodium chloride
6. extractionThe chloroform extract
7. dry with materialwas dried over sodium sulfate
8. filtrationfiltered
9. customevaporated at reduced pressure

ORD record

ord-68454836664543cfb8a8e352112bdfa3

Source dataset

uspto-grants-2016_01

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US09228053B2