Dichloromethane → HCID 67804051, compound

Participants

Reaction Steps

A 0.26 g (0.83 mmol) sample of the BOC-protected compound from step 7a was dissolved in 10 mL of 1:1 CH2Cl2 :TFA and stirred at room temperature until tlc showed no starting material. The solvent and reagent were removed by evaporation. The residue was suspended in 10% aqueous HCl, which was then adjusted to pH 12 with K2CO3, and the mixture was extracted with methylene chloride. The solvent was removed, and the residue was dried, then suspended in ether. Addition of ether/HCl precipitated the title product, which was wash with ether and dried to yield 0.62 g of the title compound. MS: 214(M+H)+, 231 (M+NH4)+, 248 (M+NH4NH3)+. NMR (D2O) δ: 1.87-2.33 (m, 4H), 3.41 (t, 2H, J=7), 4.05-4.12 (m, 2H), 4.38 (dd, 1H), 6.62-6.71 (m, 3 H). Anal. Calcd for C11H14ClF2NO.0.45 H2O: C, 51.25; H, 5.82; N 5.43; Found: C, 51.36; H, 5.35; N, 5.45.

Provenance & Evidence