Sodium Hydroxide → 2-Amino-4-methyl-thiazole-5-carboxylic acid

HRID 560533

反応式

HRID 560533 の反応式
[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

反応物 2

HCID 14798Sodium HydroxideHCID 343747Ethyl 2-amino-4-methylthiazole-5-carboxylate

生成物 1

HCID 8322432-Amino-4-methyl-thiazole-5-carboxylic acid収率 94%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

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

  1. temperaturewas heated
  2. temperatureto reflux overnight
  3. customTetrahydrofuran was removed in vacuo
  4. customThe precipitate obtained
  5. filtrationwas collected by filtration
  6. 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

関連ノート

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