Triethylamine → (4-Chloro-pyrrolo[2,1-f][1,2,4]triazin-5-ylmethyl)-triethyl-ammonium bromide
反応式
[Br:1][CH2:2][C:3]1[CH:4]=[CH:5][N:6]2[C:11]=1[C:10]([Cl:12])=[N:9][CH:8]=[N:7]2.[CH3:13][CH2:14][N:15]([CH2:18][CH3:19])[CH2:16][CH3:17]>C1COCC1>[Br-:1].[Cl:12][C:10]1[C:11]2=[C:3]([CH2:2][N+:15]([CH2:18][CH3:19])([CH2:16][CH3:17])[CH2:14][CH3:13])[CH:4]=[CH:5][N:6]2[N:7]=[CH:8][N:9]=1参加物
4
実験手順
A mixture of 5-bromomethyl-4-chloro-pyrrolo[2,1-f][1,2,4]triazine (2.7 g, 11 mmol), Et3N (5 mL, 36 mmol) in THF (20 mL) was stirred at rt for 12 h. The solid was filtered and rinsed with THF and Et2O, dried to give the desired product (3.38 g, 89%). Analytical HPLC retention time=0.776 min. (Chromolith SpeedROD 4.6×50 mm, 10–90% aqueous methanol over 4 minutes containing 0.1% TFA, 4 mL/min, monitoring at 220 nm); MS(ESI+) m/z 267 (M+H)+.
後処理
- filtrationThe solid was filtered
- washrinsed with THF and Et2O
- customdried
出典と根拠
- ORDレコード
- ord-5b3b9d4e49474c568cec840ead8f0d11
- 出典データセット
- uspto-grants-2007_02
- 特許番号
- US07173031B2
反応ノート
読み込み中…