Methanol → Methyl 4-dimethylaminobenzoate
反応式
[CH3:1][N:2]([CH3:12])[C:3]1[CH:11]=[CH:10][C:6]([C:7]([OH:9])=[O:8])=[CH:5][CH:4]=1.OS(O)(=O)=O.[CH3:18]O>>[CH3:1][N:2]([CH3:12])[C:3]1[CH:11]=[CH:10][C:6]([C:7]([O:9][CH3:18])=[O:8])=[CH:5][CH:4]=1参加物
4
実験手順
p-Dimethylaminobenzoic acid (50 g.) and concentrated H2SO4 (25 ml.) in 350 ml. methanol were refluxed 18 hours. The reaction mixture was cooled, quenched with ice and water (350 ml.), neutralized portionwise with KHCO3 until foaming ceased, and extracted 3×200 ml. CHCl3. The organic layers were combined, washed 1×150 ml. brine, dried (MgSO4) and reduced in volume to yield crystalline title product, 52 g.; 1H-nmr: 3.02 (s, 6H), 3.87 (s, 3H), 6.66 (d, J=16 Hz, 2H), 7.95 (d, J=16 Hz, 2H).
後処理
- temperatureThe reaction mixture was cooled
- customquenched with ice and water (350 ml.), neutralized portionwise with KHCO3 until foaming
- extractionextracted 3×200 ml
- washwashed 1×150 ml
- dry with materialbrine, dried (MgSO4)
出典と根拠
- ORDレコード
- ord-05b040c532f649a6a9c0789244b217ae
- 出典データセット
- uspto-grants-1988_08
- 特許番号
- US04762921
反応ノート
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