反应详情

A solution of (R)-(-)-phenylglycinol (2.20 g, 16.1 mmol) and (3R)--N-tert-butyloxycarbonyl-3-methylsulphonyloxymethylpyrrolidine (1.0 g, 3.58 mmol), in toluene (20 ml), was heated at 150° C. for 6 h in sealed pressure tube (Aldrich). The solvent was then removed under vacuum and the residue taken up into ethyl acetate (200 ml) and washed with water (×4). The organic was dried (MgSO4) and evaporated and the crude product chromatographed on silica gel eluting with CH2Cl2 /MeOH (97:3) to give the title-α-(hydroxymethyl)benzylaminomethylpyrrolidine (1.0 g, 87%), δ (360 MHz, CDCl3) 1.45 (9H, s, OC(Me)3), 1.52-2.60 (5H, m, CH2 and CH), 2.90-3.76 (7H, m, 3 of CH2 and CH), 7.25-7.39 (5H, m, Ar--H).

1. customThe solvent was then removed under vacuum
2. washwashed with water (×4)
3. dry with materialThe organic was dried (MgSO4)
4. customevaporated
5. customthe crude product chromatographed on silica gel eluting with CH2Cl2 /MeOH (97:3)