Sulfuric Acid → 6-[1,2]Oxazinan-2-yl-N,N'-dipropyl-[1,3,5]triazine-2,4-diamine hydrogen sulfate
反応式
[O:1]1[CH2:6][CH2:5][CH2:4][CH2:3][N:2]1[C:7]1[N:12]=[C:11]([NH:13][CH2:14][CH2:15][CH3:16])[N:10]=[C:9]([NH:17][CH2:18][CH2:19][CH3:20])[N:8]=1.[OH:21][S:22]([OH:25])(=[O:24])=[O:23]>>[S:22]([OH:25])([OH:24])(=[O:23])=[O:21].[O:1]1[CH2:6][CH2:5][CH2:4][CH2:3][N:2]1[C:7]1[N:12]=[C:11]([NH:13][CH2:14][CH2:15][CH3:16])[N:10]=[C:9]([NH:17][CH2:18][CH2:19][CH3:20])[N:8]=1参加物
3
実験手順
6-[1,2]Oxazinan-2-yl-N,N′-dipropyl-[1,3,5]triazine-2,4-diamine hydrogen sulfate (LVIII) was prepared from 6-[1,2]oxazinan-2-yl-N,N′-dipropyl-[1,3,5]triazine-2,4-diamine (LVII) and 95% H2SO4 as described in Example 20. Quantitative yield was isolated. 400 MHz 1H-NMR (DMSO-d6, ppm) 11.6-11.3 (1H, br s), 8.61-8.41 (0.8H, m), 8.18-8.03 (0.2H, m), 7.63-7.28 (1H, m), 4.14-4.08 (2H, m), 3.92-3.81 (2H, m, overlapped with water), 3.36-3.19 (4H, m), 1.86-1.78 (2H, m), 1.77-1.68 (2H, m), 1.6-1.45 (4H, m), 1.60-1.45 (6H, m). ESI-MS (m/z): 281 [M+H]+. M.P.: 134-137° C.
後処理
- customQuantitative yield was isolated
出典と根拠
- ORDレコード
- ord-1d9af7d1a094438fa8b472c6a8487ad8
- 出典データセット
- uspto-grants-2016_05
- 特許番号
- US09351972B2
反応ノート
読み込み中…