1-Amino-2-propanol → HCID 12384307、化合物
反応式
[NH2:1][CH2:2][CH:3]([OH:5])[CH3:4].[C:6]1(=O)[O:11][C:9](=[O:10])[C:8]2=[CH:12][CH:13]=[CH:14][CH:15]=[C:7]12.C(N(CC)CC)C.C1(C)C=CC=CC=1>O>[CH2:6]([O:11][C:9]([NH:1][CH2:2][CH:3]([OH:5])[CH3:4])=[O:10])[C:7]1[CH:8]=[CH:12][CH:13]=[CH:14][CH:15]=1参加物
6
実験手順
To a round bottom flask equipped with Dean-Stark trap was added (1) (2 g, 7.4 mmol), phthalic anhydride (1.1 g, 7.4 mmol), triethylamine (0.1 mL) and toluene (50 mL). The reaction mixture was heated to reflux and water produced was collected. After refluxing for 2 hours, the solvent was removed. The residue was acidified using 1 N HCl, filtered and washed with water, dried to give 2.2 g of (2). 1H NMR (DMSO-d6, 400 MHz): δ 7.8 (m, 4H), 7.3 (m, 5H), 7.1 (d, 2H), 6.8 (d, 2H), 5.05 (m, 1H), 3.3 (m, 2H).
後処理
- customTo a round bottom flask equipped with Dean-Stark trap
- temperatureThe reaction mixture was heated
- temperatureto reflux
- customwas collected
- temperatureAfter refluxing for 2 hours
- customthe solvent was removed
- filtrationfiltered
- washwashed with water
- customdried
出典と根拠
- ORDレコード
- ord-2b99da6e97b8436a8959456d82cfddc4
- 出典データセット
- uspto-grants-2009_03
- 特許番号
- US07511063B2
反応ノート
読み込み中…