Isoamylamine → HCID 2802345, compound

To a solution of 3-methylbutylamine (20 g, 229 mmol) in 840 ml of dichloromethane were added 35.6 ml triethylamine (255 mmol) and 28.8 ml of phenyl chloroformate (230 mmol) at 0° C. The mixture was stirred for three hours at room temperature. After distilling off the solvent under reduced pressure, 200 ml of ethyl acetate and 200 ml of water were added to the residue. The organic layers were separated and water layer was extracted with ethyl acetate (100 ml×3). The organic layers were combined, washed with water and saturated sodium chloride solution successively and dried over magnesium sulfate. The solvent was distilled off and the crystals separated out were collected by filtration, and washed with petroleum ether to give 39.5 g of phenyl 3-methylbutylcarbamate (83%) as colorless crystals.

1. distillationAfter distilling off the solvent under reduced pressure, 200 ml of ethyl acetate and 200 ml of water
2. additionwere added to the residue
3. customThe organic layers were separated
4. extractionwater layer was extracted with ethyl acetate (100 ml×3)
5. washwashed with water and saturated sodium chloride solution successively
6. dry with materialdried over magnesium sulfate
7. distillationThe solvent was distilled off
8. customthe crystals separated out
9. filtrationwere collected by filtration
10. washwashed with petroleum ether

ORD record

ord-3437f26b54f14020af511bd403cd87c2

Source dataset

uspto-grants-1995_11

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05466820