Acetic Anhydride → HCID 19028813, compound

In formic acid (100 ml) was dissolved 4-amino-3,3-diphenylbutanol (reference compound 7-1) (17.1 g) followed by addition of acetic anhydride (16 ml) and the mixture was stirred at room temperature for 7 hours. The reaction mixture was concentrated to dryness and the residue was distributed between chloroform and water. The aqueous layer was made basic with aqueous ammonia and extracted with chloroform. The extract was dried over anhydrous sodium sulfate and concentrated to dryness. The residue was dissolved in ethanol (50 ml) and the solution was stirred with 1N-sodium hydroxide solution (60 ml) at room temperature for 15 minutes. To this reaction mixture was added water and the resulting crystals were recovered by filtration. The crystals were washed serially with water and ethyl acetate to provide the title compound (16 g) as colorless powder.

1. concentrationThe reaction mixture was concentrated to dryness
2. extractionextracted with chloroform
3. dry with materialThe extract was dried over anhydrous sodium sulfate
4. concentrationconcentrated to dryness
5. dissolutionThe residue was dissolved in ethanol (50 ml)
6. stirringthe solution was stirred with 1N-sodium hydroxide solution (60 ml) at room temperature for 15 minutes
7. additionTo this reaction mixture was added water
8. filtrationthe resulting crystals were recovered by filtration
9. washThe crystals were washed serially with water and ethyl acetate

ORD record

ord-7b476a1fe7054562aceb5256a59b75d0

Source dataset

uspto-grants-1997_08

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05654296