反应详情

A 4 M dioxane solution of HCl (0.50 mL) was added to a methanol (1 mL) solution of 1-(3-amino-4-hydroxybenzyl)-4-[[N-(2-(tert-butoxycarbonylamino)-4,5-difluorobenzoyl)glycyl]aminomethyl]piperidine (20.0 mg, 0.035 mmol), and the resulting mixture was stirred at room temperature overnight and concentrated. The obtained residue was then dissolved in methanol, loaded onto a Varian™ SCX column, washed with methanol (5 mL×2), eluted with a 2 M methanol solution of NH3 (5 mL) and concentrated to thereby afford 4-[[N-(2-amino-4,5-difluorobenzoyl)glycyl]aminomethyl]-1-(3-amino-4-hydroxybenzyl)piperidine (Compd. No. 2141) (17.6 mg, quantitative). The purity was determined by RPLC/MS (85%). ESI/MS m/e 448.3 (M++H, C22H27F2N5O3).

1. concentrationconcentrated
2. dissolutionThe obtained residue was then dissolved in methanol
3. washwashed with methanol (5 mL×2)
4. washeluted with a 2 M methanol solution of NH3 (5 mL)
5. concentrationconcentrated to thereby afford 4-[[N-(2-amino-4,5-difluorobenzoyl)glycyl]aminomethyl]-1-(3-amino-4-hydroxybenzyl)piperidine (Compd. No