Sodium Hydroxide → 2-Amino-4-methyl-thiazole-5-carboxylic acid
反応式
[NH2:1][C:2]1[S:3][C:4]([C:8]([O:10]CC)=[O:9])=[C:5]([CH3:7])[N:6]=1.[OH-].[Na+]>O1CCCC1.O>[NH2:1][C:2]1[S:3][C:4]([C:8]([OH:10])=[O:9])=[C:5]([CH3:7])[N:6]=1参加物
5
実験手順
A mixture of ethyl 2-amino-4-methylthiazole-5-carboxylate (6.58 g, 35.5 mmol) and NaOH (5.40 g, 135 mmol) in tetrahydrofuran (60 mL) and water (30 mL) was heated to reflux overnight. Tetrahydrofuran was removed in vacuo, and the residue was neutralized with 5% hydrochloric acid solution to pH 5˜6. The precipitate obtained was collected by filtration and dried to afford the crude 2-amino-4-methylthiazole-5-carboxylic acid (5.20 g, 94%): 1H NMR (300 MHz, DMSO-d6) δ 7.63 (s, 2H), 2.30 (s, 3H); MS (ES+) m/z 159.1 (M+1).
後処理
- temperaturewas heated
- temperatureto reflux overnight
- customTetrahydrofuran was removed in vacuo
- customThe precipitate obtained
- filtrationwas collected by filtration
- customdried
出典と根拠
- ORDレコード
- ord-45fc3713ccff472292b5824c2dd98953
- 出典データセット
- uspto-grants-2011_11
- 特許番号
- US08063084B2
反応ノート
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