Hydrochloric Acid → 2-[(4-formyl-1,3-dimethyl-1H-pyrazol-5-yl)sulfanyl]acetic acid

HRID 534817ノート

反応式

HRID 534817 の反応式
[CH:1]([C:3]1[C:4]([CH3:16])=[N:5][N:6]([CH3:15])[C:7]=1[S:8][CH2:9][C:10]([O:12]CC)=[O:11])=[O:2].[OH-].[Na+].CO.Cl>O1CCCC1>[CH:1]([C:3]1[C:4]([CH3:16])=[N:5][N:6]([CH3:15])[C:7]=1[S:8][CH2:9][C:10]([OH:12])=[O:11])=[O:2]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 887MethanolHCID 14798Sodium HydroxideHCID 63802037Ethyl [(4-formyl-1,3-dimethyl-1H-pyrazol-5-yl)sulfanyl]acetate

生成物 1

HCID 470023932-[(4-formyl-1,3-dimethyl-1H-pyrazol-5-yl)sulfanyl]acetic acid収率 58%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

A mixture of ethyl [(4-formyl-1,3-dimethyl-1H-pyrazol-5-yl)sulfanyl]acetate obtained in Reference Example 2 (2.12 g), 8 M sodium hydroxide solution (5 mL), methanol (50 mL), and tetrahydrofuran (50 mL) was stirred at room temperature for 2 h. 6 M Hydrochloric acid solution was added to the reaction solution, and the mixture was extracted with ethyl acetate. The ethyl acetate layer was washed with saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure, and the residue was recrystallized from ethyl acetate-diisopropyl ether to provide the title compound (1.09 g, 58%) as a solid.

後処理

  1. extractionthe mixture was extracted with ethyl acetate
  2. washThe ethyl acetate layer was washed with saturated brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. customThe solvent was evaporated under reduced pressure
  5. customthe residue was recrystallized from ethyl acetate-diisopropyl ether

出典と根拠

ORDレコード
ord-fd99a6f0705d4451a3c57a118e994a34
出典データセット
uspto-grants-2014_10
特許番号
US08853215B2

反応ノート

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