2-(3-Chloropropyl)-2-methyl-1,3-dioxolane → HCID 10887910, compound

5-Chloro-2-pentanone ethylene ketal (5.0 g, 30.4 mmol) was stirred in DMF with lithium azide (5.95 g, 120 mmol) at 60° C. for 48 hrs. The mixture was evaporated to dryness. The product was then dissolved in toluene (50 ml) and washed with water (3×15 ml). The organic phase was evaporated and the resulting 5-azido-2-pentanone ethylene ketal was stirred in 50 ml of 70% trifluoroacetic acid for 24 hrs. The reaction mixture was neutralized with sodium bicarbonate and extracted with ethyl acetate. The organic phase was dried over magnesium sulfate and evaporated to yield the desired ketone as an oil.

1. customThe mixture was evaporated to dryness
2. dissolutionThe product was then dissolved in toluene (50 ml)
3. washwashed with water (3×15 ml)
4. customThe organic phase was evaporated
5. extractionextracted with ethyl acetate
6. dry with materialThe organic phase was dried over magnesium sulfate
7. customevaporated

ORD record

ord-968f8f3ae92a47c6a52a5c8336d36a90

Source dataset

uspto-grants-1998_07

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05775329