反应详情

(S)-(1-{4-[Bis-(4-fluoro-phenyl)-methyl]-piperazin-1-ylmethyl}-3-methyl-butyl)carbamic acid tert-butyl ester (0.225 g, 0.461 mmol, Example 35) was dissolved in CH2Cl2 (4 mL) under nitrogen at ambient temperature. To this solution was added trifluoroacetic acid (0.5 mL). The resulting reaction mixture was stirred for 3 hours, then concentrated in vacuo. The viscous pale-amber oil obtained was dissolved in 5 mL of ether and treated with 3.3 mL of saturated ethereal HCl. The resulting white precipitate was triturated with 3:1 EtOAc/2,2,4-trimethylpentane, and collected via filtration. The filtrate was concentrated in vacuo affording a viscous amber oil (189 mg) which was used in the subsequent reaction without further purification.

1. customThe resulting reaction mixture
2. concentrationconcentrated in vacuo
3. customThe viscous pale-amber oil obtained
4. customThe resulting white precipitate was triturated with 3:1 EtOAc/2,2,4-trimethylpentane
5. filtrationcollected via filtration
6. concentrationThe filtrate was concentrated in vacuo