Ethyl trifluoroacetate → 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レコード

ord-eccf39775a9b415b9741c6b119369bd0

出典データセット

uspto-grants-2013_05

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08440689B2