Hydrochloric Acid → 5-Methyl-4-oxo-2-(thiophen-3-ylmethyl)-3,4-dihydrothieno[2,3-d]pyrimidine-6-carboxylic acid

HRID 388405

反応式

HRID 388405 の反応式
[CH3:1][C:2]1[C:10]2[C:9](=[O:11])[NH:8][C:7]([CH2:12][C:13]3[CH:17]=[CH:16][S:15][CH:14]=3)=[N:6][C:5]=2[S:4][C:3]=1[C:18]([O:20]CC)=[O:19].[OH-].[Na+].Cl>C(O)C>[CH3:1][C:2]1[C:10]2[C:9](=[O:11])[NH:8][C:7]([CH2:12][C:13]3[CH:17]=[CH:16][S:15][CH:14]=3)=[N:6][C:5]=2[S:4][C:3]=1[C:18]([OH:20])=[O:19]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 68664667Ethyl 5-methyl-4-oxo-2-(thiophen-3-ylmethyl)-3,4-dihydrothieno[2,3-d]pyrimidine-6-carboxylate

生成物 1

HCID 160910835-Methyl-4-oxo-2-(thiophen-3-ylmethyl)-3,4-dihydrothieno[2,3-d]pyrimidine-6-carboxylic acid収率 92.2%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A mixture of 379 mg of ethyl 5-methyl-4-oxo-2-(thiophen-3-ylmethyl)-3,4-dihydrothieno[2,3-d]pyrimidine-6-carboxylate as synthesized in Production Example 1, 3.4 mL of 1N aqueous sodium hydroxide solution and 2.2 mL of ethanol was heated under reflux for 2 hours. After cooling off, the reaction liquid was poured on ice, rendered acidic with diluted hydrochloric acid, and the precipitated crystals were recovered by filtration. After washing with water, the crystals were dried by heating under reduced pressure, to provide 320 mg of 5-methyl-4-oxo-2-(thiophen-3-ylmethyl)-3,4-dihydrothieno[2,3-d]pyrimidine-6-carboxylic acid.

後処理

  1. temperaturewas heated
  2. temperatureunder reflux for 2 hours
  3. temperatureAfter cooling off
  4. customthe reaction liquid
  5. additionwas poured on ice
  6. filtrationthe precipitated crystals were recovered by filtration
  7. washAfter washing with water
  8. customthe crystals were dried
  9. temperatureby heating under reduced pressure

出典と根拠

ORDレコード
ord-bdef864c039d47bc9d99340187e10c79
出典データセット
uspto-grants-2013_02
特許番号
US08377944B2

関連ノート

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