三氟乙酸乙酯 → Acetamide, N-(2-aminocyclohexyl)-2,2,2-trifluoro-, cis-

cis-Cyclohexane-1,2-diamine (5.00 g, 43.9 mmol, 1.00 eq) was charged to a 250 mL three-neck round bottom flask equipped with an overhead stirrer and a thermocouple. Ethanol (50 mL) was added and the solution was cooled to <0° C. using an ice-brine bath. A solution of ethyl trifluoroacetate (6.23 g, 1.00 eq) in EtOH (25 mL) was added via a syringe pump over a one hour period. Once the addition was complete, the cooling bath was removed and the solution was slowly warmed to RT and stirred for 3.5 hours to afford the title compound in EtOH. Half (41 mL, about 21.9 mmol) of the total solution (about 82 mL) was carried into the next step.

1. customequipped with an overhead stirrer
2. temperaturethe solution was cooled to <0° C.
3. additionOnce the addition
4. customthe cooling bath was removed

ORD记录

ord-ad0d059b0c884f9ea153fc014d040e82

来源数据集

uspto-grants-2015_08

DOI

10.6084/m9.figshare.5104873.v1

专利号

US09108970B2