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Potassium Hydroxide → 2-(Methoxymethyl)-4-methyl-1,3-thiazole-5-carboxylic acid

HRID 248420
ノート
印刷プレビュー

反応式

HRID 248420 の反応式
[OH-].[K+].C([O:5][C:6]([C:8]1[S:12][C:11]([CH2:13][O:14][CH3:15])=[N:10][C:9]=1[CH3:16])=[O:7])C>C(O)C>[CH3:15][O:14][CH2:13][C:11]1[S:12][C:8]([C:6]([OH:7])=[O:5])=[C:9]([CH3:16])[N:10]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 14797Potassium HydroxideHCID 53930828HCID 53930828、化合物

生成物 1

HCID 200880752-(Methoxymethyl)-4-methyl-1,3-thiazole-5-carboxylic acid

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

6.7 g of 85% potassium hydroxide in 100 ml of ethanol are added at room temperature to 22.1 g of 2-methoxymethyl-4-methylthiazole-5-carboxylic acid ethyl ester and the reaction mixture is then heated under reflux for 18 hours. After cooling, the ethanol is evaporated off and the residue is dissolved in 200 ml of water. After stirring with active carbon, the mixture is filtered over Hyflo and the filtrate is acidified with concentrated hydrochloric acid with vigorous stirring. The resulting yellowish crystals are filtered off, washed with water and dried. After recrystallisation from tetrahydrofuran/petroleum ether (30°-45° C.) (=10:1) the yellowish crystals melt at 168°-169.5° C.

後処理

  1. temperaturethe reaction mixture is then heated
  2. temperatureunder reflux for 18 hours
  3. temperatureAfter cooling
  4. customthe ethanol is evaporated off
  5. dissolutionthe residue is dissolved in 200 ml of water
  6. filtrationthe mixture is filtered over Hyflo
  7. filtrationThe resulting yellowish crystals are filtered off
  8. washwashed with water
  9. customdried
  10. customAfter recrystallisation from tetrahydrofuran/petroleum ether (30°-45° C.) (=10:1) the yellowish crystals
  11. custommelt at 168°-169.5° C.

出典と根拠

ORDレコード
ord-c45df4e6d14646bfb3a918a2f45cdc13
出典データセット
uspto-grants-1993_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05210205

反応ノート

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