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

HRID 244625ノート

反応式

HRID 244625 の反応式
[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

参加物

5

反応物 2

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

生成物 1

HCID 150939445-Isopropyl-2-methylthiazole-4-carboxylic acid収率 98.4%

試薬・触媒・溶媒 2

HCID 313Hydrochloric Acid触媒HCID 312751,4-Dioxane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-a67bd060ef314631bd504549663bad36
出典データセット
uspto-grants-2014_02
特許番号
US08658635B2

反応ノート

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