反应详情

温度

25 °C

To a mixture of 1.1 g of N-phenylmethyloxycarbonyl proline TDO-ester (Cf Hollitzer, Seewald and Steglichm Ang. Int. Edit. 1976, Vol. 15, 444) and 0.42 g of 3-amino-1,1,1-trifluoro-4-methyl-2-pentanol hydrochloride in 50 ml of CH2Cl2 was added dropwise 0.40 g of triethylamine. After stirring for 14 hours at 25° C., aqueous KHSO4 was added, the layers separated and the organic layer washed with aqueous KHSO4, aqueous KHCO3, H2O and then brine (2x). After drying (MgSO4), solvents were flash evaporated to yield 0.54 g of a solid residue which was recrystallized in Et20 to give 0.24 g of the analytically pure expected amide; m.p. 99° C.

1. customthe layers separated
2. washthe organic layer washed with aqueous KHSO4, aqueous KHCO3, H2O
3. dry with materialAfter drying (MgSO4), solvents
4. customevaporated