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

HRID 560533

반응식

HRID 560533 반응식
[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

참가 물질

5

반응물 2

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

생성물 1

HCID 8322432-Amino-4-methyl-thiazole-5-carboxylic acid수율 94%

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매

실험 절차

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).

후처리

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

출처 및 근거

ORD 기록
ord-45fc3713ccff472292b5824c2dd98953
출처 데이터셋
uspto-grants-2011_11
특허 번호
US08063084B2

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