Dimethylamine → HCID 11676128、化合物

反応式

[CH3:1][O:2][C:3]1[CH:4]=[C:5]([NH:9][C:10]2[C:19]3[C:14](=[CH:15][CH:16]=[CH:17][C:18]=3[CH2:20][N:21]3[CH2:26][CH2:25][C@@H:24]([NH:27]C(=O)OCC=C)[C@H:23]([C:34](=[O:37])[NH:35][CH3:36])[CH2:22]3)[N:13]=[CH:12][N:11]=2)[CH:6]=[CH:7][CH:8]=1.N(C)C>C1COCC1.C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1>[NH2:27][C@@H:24]1[CH2:25][CH2:26][N:21]([CH2:20][C:18]2[CH:17]=[CH:16][CH:15]=[C:14]3[C:19]=2[C:10]([NH:9][C:5]2[CH:6]=[CH:7][CH:8]=[C:3]([O:2][CH3:1])[CH:4]=2)=[N:11][CH:12]=[N:13]3)[CH2:22][C@H:23]1[C:34]([NH:35][CH3:36])=[O:37]

参加物

実験手順

A solution of 15E (27 mg, 0.054 mmol) in THF (3 ml) was degassed and purged with N2. To this was added 2N Me2NH in THF (95 μl, 0.19 mmol), followed by Pd(PPh3)4 (9 mg, 0.0078 mmol). The mixture was stirred at room temperature for 1.5 h. Concentration in vacuo followed by purification using preparative HPLC gave, after concentration and lyophilization, a TFA salt of 15F (20.3 mg, 70%) as a solid. The compound has an analytical HPLC retention time=1.307 min (Chromolith SpeedROD column 4.6×50 mm, 10-90% aqueous methanol containing 0.1% TFA over 4 minutes, 4 mL/min, monitoring at 254 nm) and a LC/MS M++H=421+.