Ethanamine, 2,2,2-trifluoro- → HCID 89967335, 화합물

To a dioxane (1 mL) solution of 2,2,2-trifluoroethanamine (80 mg, 0.81 mmol) and DIEA (0.28 mL, 1.6 mmol) at 0° C. was added benzyl (2-(chlorosulfonyl)ethyl)carbamate (150 mg, 0.54 mmol) in acetonitrile (1 mL). The reaction was allowed to reach room temperature over a period of 20 minutes. The reaction mixture was concentrated under reduced pressure, and the residue purified using reverse phase HPLC (YMC Sunfire 5u (C18) 30×100 mm, 0-100% ACN (90% in H2O, 0.1% TFA) using gradient over 16 min with flow rate 40 mL/min and UV detection at 220 nm) to give Compound B30a (95 mg, 39% yield). HPLC: RT=3.84 (LCMS Method M). MS (ES): m/z=340.9 [M+H]+. 1H NMR (500 MHz, CHLOROFORM-d) d 7.43-7.34 (m, 5H), 5.28 (br. s., 2H), 5.15 (s, 2H), 3.86-3.68 (m, 4H), 3.35-3.24 (m, 2H).

1. concentrationThe reaction mixture was concentrated under reduced pressure
2. customthe residue purified
3. customphase HPLC (YMC Sunfire 5u (C18) 30×100 mm, 0-100% ACN (90% in H2O, 0.1% TFA) using gradient over 16 min with flow rate 40 mL/min and UV detection at 220 nm)
4. customto give Compound B30a (95 mg, 39% yield)
5. customRT=3.84 (LCMS Method M)

ORD 기록

ord-3cfb5d9d3e1c41ad9174fb5dc8294c50

출처 데이터셋

uspto-grants-2015_03

DOI

10.6084/m9.figshare.5104873.v1

특허 번호

US08987314B2