Trifluoroacetic acid → HCID 55288816, Verbindung

To a stirred solution of (3RS,4R)-2-methyl-4-(trityl-amino)-hexan-3-ol (0.53 g, 1 eq, 1.41 mmol) in DCM (20 mL) under an argon atmosphere at room temperature, was added CF3COOH (5 mL) dropwise, and the solution was stirred at this temperature for 1 h. The solvent was evaporated in vacuo, the residue was precipitated from Et2O (10 mL) with hexane (90 mL) with stirring to give a yellow oil. The solvent was decanted from the oil, and the oil was washed with hexane (20 mL) and dried in vacuo to afford the title compound as a light yellow oil. Yield: 0.18 g (100%). (50% de 3S,4R: 50% de 3R,4R). 1H-NMR (d6-DMSO, 250 MHz): δ 0.85-0.99 (m, 9H, NH2CH (CH2CH3)CH(CH(CH2)OH;, 1.42-1.79 (m, 2H, NH2CH(CH2CH3)CH (CH(CH3)2) OH), 2.95 (m, 1H, NH2CH(CH2CH3)CH(CH(CH3)2)OH), 3.18 (m, 1H, NH2CH (CH2CH3)CH(H(CH(CH3)2)OH), 3.37 (m, 1H, NH2CH(CH2CH3)CH(CH(CH3)2)OH, 7.58 (bs, 2H, NH2CH(CH2CH3)CH(CH(CH3)2)OH).

1. customThe solvent was evaporated in vacuo
2. customthe residue was precipitated from Et2O (10 mL) with hexane (90 mL)
3. stirringwith stirring
4. customto give a yellow oil
5. customThe solvent was decanted from the oil
6. washthe oil was washed with hexane (20 mL)
7. customdried in vacuo

ORD-Eintrag

ord-6910cf75a344499993fd3418a5fa804b

Quelldatensatz

uspto-grants-2009_06

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US07544689B2