Methyl iodide → HCID 58550842、化合物

反応式

[CH3:1]I.[CH2:3]([C:5]1[CH:10]=[CH:9][C:8]([C:11]([N:13]2[CH2:32][CH2:31][C:16]3([C:21]4=[CH:22][CH:23]=[CH:24][N:20]4[C:19]4[CH:25]=[CH:26][C:27]([CH2:29][OH:30])=[CH:28][C:18]=4[O:17]3)[CH2:15][CH2:14]2)=[O:12])=[CH:7][C:6]=1[O:33][CH3:34])[CH3:4].[H-].[Na+]>CN(C=O)C>[CH2:3]([C:5]1[CH:10]=[CH:9][C:8]([C:11]([N:13]2[CH2:14][CH2:15][C:16]3([O:17][C:18]4[CH:28]=[C:27]([CH2:29][O:30][CH3:1])[CH:26]=[CH:25][C:19]=4[N:20]4[CH:24]=[CH:23][CH:22]=[C:21]34)[CH2:31][CH2:32]2)=[O:12])=[CH:7][C:6]=1[O:33][CH3:34])[CH3:4]

参加物

実験手順

MeI (7.2 μL, 0.12 mmol) was added to a solution of (4-ethyl-3-methoxy-phenyl)-[7′-(hydroxymethyl)spiro[piperidine-4,4′-pyrrolo[2,1-c][1,4]benzoxazine]-1-yl]methanone (50 mg, 0.12 mmol) and NaH (4.6 mg, 0.12 mmol) in DMF (1 mL) and was stirred at room temperature for 1 hour. The reaction was filtered and purified by reverse phase LC-MS (10-99% CH3CN/H2O). Pure fractions were combined and evaporated to yield (4-ethyl-3-methoxyphenyl)(7-(methoxymethyl)spiro[benzo[b]pyrrolo[1,2-d][1,4]oxazine-4,4′-piperidine]1′-yl)methanone. ESI-MS m/z calc. 446.5. found 447.5 (M+1)+; Retention time: 2.11 minutes (3 min run).