1,2-Dichloroethane → tert-Butyl {2-[(1-hydroxy-2-methylpropan-2-yl)amino]-2-oxo-1-[3-(trifluoromethyl)phenyl]ethyl}-carbamate

360 mg (1.88 mmol) of EDC were added to a mixture of 400 mg (1.25 mmol) of [(tert-butoxycarbonyl)amino][3-(trifluoromethyl)phenyl]acetic acid and 254 mg (1.88 mmol) of HOBt in 10 ml of DMF, and the mixture was stirred at RT for 20 min. The resulting solution was added dropwise to a solution of 168 mg (1.88 mmol) of 2-amino-2-methyl-1-propanol in 2 ml of DMF. The reaction mixture was stirred at RT for 20 min. For purification, 1 ml of 1N hydrochloric acid was added and the entire reaction mixture was separated by preparative HPLC [Method 6]. The appropriate fraction was concentrated on a rotary evaporator and the residue was dried under high vacuum. This gave 364 mg (74% of theory) of the title compound.

1. stirringThe reaction mixture was stirred at RT for 20 min
2. customFor purification, 1 ml of 1N hydrochloric acid
3. additionwas added
4. customthe entire reaction mixture
5. customwas separated by preparative HPLC [Method 6]
6. concentrationThe appropriate fraction was concentrated on a rotary evaporator
7. customthe residue was dried under high vacuum

ORD-Eintrag

ord-bb5dc7cceb034d738b5f7ca68756e82f

Quelldatensatz

uspto-grants-2015_05

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US09034855B2