Hydrochloric Acid → 5-Isopropyl-2-methylthiazole-4-carboxylic acid

HRID 244625노트

반응식

HRID 244625 반응식
[CH3:1][C:2]1[S:3][C:4]([CH:12]([CH3:14])[CH3:13])=[C:5]([C:7]([O:9]CC)=[O:8])[N:6]=1.Cl>O1CCOCC1.Cl>[CH3:1][C:2]1[S:3][C:4]([CH:12]([CH3:14])[CH3:13])=[C:5]([C:7]([OH:9])=[O:8])[N:6]=1

참가 물질

5

반응물 2

HCID 313Hydrochloric AcidHCID 58356351Ethyl 2-methyl-5-(1-methylethyl)-1,3-thiazole-4-carboxylate

생성물 1

HCID 150939445-Isopropyl-2-methylthiazole-4-carboxylic acid수율 98.4%

시약·촉매·용매 2

HCID 313Hydrochloric Acid촉매HCID 312751,4-Dioxane용매

실험 절차

Ethyl 2-methyl-5-(1-methylethyl)-1,3-thiazole-4-carboxylate (200 mg) was dissolved in 1,4-dioxane (2 ml). Hydrochloric acid (2 ml) was added and the mixture was heated at reflux under nitrogen for 18 h. One drop of concentrated hydrochloric acid was added and the mixture was heated at reflux for 72 h. The mixture was cooled to RT, the solvent was removed in vacuo and toluene (15 ml) was added. The solvent was removed in vacuo to give a brown oil which solidified on standing. The product was dried in a vacuum oven overnight to give the title compound (171 mg) as a brown solid.

후처리

  1. temperaturethe mixture was heated
  2. temperatureat reflux under nitrogen for 18 h
  3. temperaturethe mixture was heated
  4. temperatureat reflux for 72 h
  5. customthe solvent was removed in vacuo and toluene (15 ml)
  6. additionwas added
  7. customThe solvent was removed in vacuo
  8. customto give a brown oil which
  9. customThe product was dried in a vacuum oven overnight

출처 및 근거

ORD 기록
ord-a67bd060ef314631bd504549663bad36
출처 데이터셋
uspto-grants-2014_02
특허 번호
US08658635B2

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