(2-(2-(Dimethylamino)ethylamino)-3-fluorophenyl)methanol → 2-(2-(Dimethylamino)ethylamino)-3-fluorobenzaldehyde
反応式
[CH3:1][N:2]([CH3:15])[CH2:3][CH2:4][NH:5][C:6]1[C:11]([F:12])=[CH:10][CH:9]=[CH:8][C:7]=1[CH2:13][OH:14]>C1(C)C=CC=CC=1.O=[Mn]=O>[CH3:1][N:2]([CH3:15])[CH2:3][CH2:4][NH:5][C:6]1[C:11]([F:12])=[CH:10][CH:9]=[CH:8][C:7]=1[CH:13]=[O:14]参加物
4
実験手順
(2-(2-(dimethylamino)ethylamino)-3-fluorophenyl)methanol (536 mg, 2.525 mmol) and MnO2 (878.1 mg, 174.7 μL, 10.10 mmol) were heated to reflux in toluene (13 mL) overnight. The suspension was filtered through Celite with CH2Cl2 and concentrated on a rotary evaporator. The crude product was purified on 12 g Redisep ISCO column eluting with 4-55% EtOAc/Hexanes over 30 CV. 2-(2-(Dimethylamino)ethylamino)-3-fluorobenzaldehyde was identified by 1H-NMR and carried on to next reaction.
後処理
- filtrationThe suspension was filtered through Celite with CH2Cl2
- concentrationconcentrated on a rotary evaporator
- customThe crude product was purified on 12 g Redisep ISCO column
- washeluting with 4-55% EtOAc/Hexanes over 30 CV
- customcarried on to next reaction
出典と根拠
- ORDレコード
- ord-05d0d4d99adb4fb5b23619958368f273
- 出典データセット
- uspto-grants-2012_04
- 特許番号
- US08163737B2
反応ノート
読み込み中…