3-氨基-2-甲基丙醇

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: This compound was prepared from ethyl 7-[(4-fluorophenyl)methyl]-4-hydroxy-2-oxo-1-[2-(2-oxo-1-piperidinyl)ethyl]-1,2-dihydro-1,5-naphthyridine-3-carboxylate and 3-amino-2-methyl-1-propanol using methods similar to Example 563 to provide an orange solid: 1H NMR (300 MHz, DMSO-d6) δ ppm 0.89 (d, J=6.95 Hz, 3 H), 1.52-1.65 (m, 4 H), 1.79-1.88 (m, 1 H), 2.03 (t, J=6.00 Hz, 2 H), 3.20-3.47 (m, 6 H), 3.51 (t, J=6.00 Hz, 2 H), 4.16 (s, 2 H), 4.40 (t, J=6.11 Hz, 2 H), 4.64 (s, 1 H), 7.11-7.17 (m, 2 H), 7.38-7.43 (m, 2 H), 8.20 (d, J=1.47 Hz, 1 H), 8.56 (d, J=1.47 Hz, 1 H), 10.38 (t, J=5.90 Hz, 1 H), 17.24 (s, 1 H); ES+ MS: 511 (M+H+). to provide an orange solid

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: This compound was prepared from ethyl 7-[(4-fluorophenyl)methyl]-4-hydroxy-2-oxo-1-[2-(2-oxo-1-piperidinyl)ethyl]-1,2-dihydro-1,5-naphthyridine-3-carboxylate and 3-amino-2-methyl-1-propanol using methods similar to Example 563 to provide an orange solid: 1H NMR (300 MHz, DMSO-d6) δ ppm 0.89 (d, J=6.95 Hz, 3 H), 1.52-1.65 (m, 4 H), 1.79-1.88 (m, 1 H), 2.03 (t, J=6.00 Hz, 2 H), 3.20-3.47 (m, 6 H), 3.51 (t, J=6.00 Hz, 2 H), 4.16 (s, 2 H), 4.40 (t, J=6.11 Hz, 2 H), 4.64 (s, 1 H), 7.11-7.17 (m, 2 H), 7.38-7.43 (m, 2 H), 8.20 (d, J=1.47 Hz, 1 H), 8.56 (d, J=1.47 Hz, 1 H), 10.38 (t, J=5.90 Hz, 1 H), 17.24 (s, 1 H); ES+ MS: 511 (M+H+). to provide an orange solid

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: By using 3-amino-2-methylpropan-1-ol (0.10 g, 1.1 mmol), ethyl glyoxylate (polymer type, a solution of 47% toluene) (2.0 mL, 9.7 mmol) and 5-methyl-2-(2H-1,2,3-triazol-2-yl)benzoic acid (0.5 g, 2.5 mmol), the same procedure as in Reference Example 1 was carried out to obtain the title compound (0.13 g) (colorless oil).

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A solution of 3-amino-2-methyl propan-1-ol (4) (0.400 g) in dry benzene (10 ml) was treated with cyclohexanone (0.450 g) and heated at reflux in an apparatus with provision for water removal for 5 hours. The product was concentrated to give the crude 3-methyl-1-oxa-5-azospiro[5.5]undecane (5) as a yellow oil; νmax. (CH2Cl2) 3450, 1660 (weak, Schiffs base); 1460, 1450, 1160, 1040 cm-1. This material was redissolved in dry benzene (10 ml) and stirred and cooled in an ice-bath, treated with diketene (0.37 ml) and stirring continued at 0° C. for 1 h followed by room temperature for 1 h. The solvent was evaporated and the residue chromatographed on Kieselgel 60 (<230 mesh ASTM) eluting with hexane grading to 1:1 ethyl acetate/hexane, to give 1-[3-methyl-1-oxa-5-azaspiro[5.5]undecan-5-yl]butan-1,3 -dione (6) (0.400 g) as a yellow oil; νmax (CH2Cl2) 1725, 1640, 1450, 1410, 1550 cm-1 ; δ (ppm, CDCl3) 0.96 (3H, d, J=7 Hz, CH3CH); 1.25-2.70 (10H, m, cyclohexyl); 2.10-2.20 (1H, m, CH3CH); 2.27 (3H, s, C(O)CH3); 3.10 (1H, dd, J=12, 7 Hz, CHaHbN); 3.27 (1H, dd, J=11, 7 Hz, CHaHbO); 3.34 (1H, dd, J=12, 7 Hz, CHAHb N); 3.50 (2H, d, J=2.5 Hz, COCH2CO); 3.94 (1H, dd, J=11, 7 Hz, CHaHbO). heated The product was concentrated to give the crude 3-methyl-1-oxa-5-azospiro[5.5]undecane (5) as a yellow oil cooled in an ice-bath stirring followed by room temperature for 1 h The solvent was evaporated the residue chromatographed on Kieselgel 60 (<230 mesh ASTM) eluting with hexane grading to 1:1 ethyl acetate/hexane