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Hydrochloric Acid → 5-Methyl-1,3-thiazole-4-carboxylic acid

HRID 1663671
ノート
印刷プレビュー

反応式

HRID 1663671 の反応式
[CH3:1][C:2]1[S:6][CH:5]=[N:4][C:3]=1[C:7]([O:9]C)=[O:8].[OH-].[Na+].Cl>CO>[CH3:1][C:2]1[S:6][CH:5]=[N:4][C:3]=1[C:7]([OH:9])=[O:8]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 37818647Methyl 5-methyl-1,3-thiazole-4-carboxylate

生成物 1

HCID 141093205-Methyl-1,3-thiazole-4-carboxylic acid収率 50.1%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a solution of methyl 5-methyl-1,3-thiazole-4-carboxylate (1.17 g, 7.4 mmol) in methanol (15 mL) was added 8N aqueous sodium hydroxide solution (2.00 mL), and the mixture was stirred at room temperature for 18 hr. 6N Hydrochloric acid (2.67 mL) was added to the mixture, and the mixture was concentrated under reduced pressure. Water was added to the residue, and the precipitate was collected by filtration, and washed with water. The precipitate was suspended in a mixed solvent of ethyl acetate (9 mL) and ethanol (1 mL), and the mixture was stirred at 80° C. for 3 min. After allowing to cool to room temperature, the precipitate was collected by filtration, washed with ethyl acetate, and dried under reduced pressure to give the title compound (531 mg, yield 50%) as a pale-yellow solid.

後処理

  1. concentrationthe mixture was concentrated under reduced pressure
  2. additionWater was added to the residue
  3. filtrationthe precipitate was collected by filtration
  4. washwashed with water
  5. stirringthe mixture was stirred at 80° C. for 3 min
  6. temperatureto cool to room temperature
  7. filtrationthe precipitate was collected by filtration
  8. washwashed with ethyl acetate
  9. customdried under reduced pressure

出典と根拠

ORDレコード
ord-dbc7f19720f14088a12e2bfba1ad64ec
出典データセット
uspto-grants-2011_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08034812B2

反応ノート

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