Water → 2-(Hydroxymethyl)pyrazolo[1,5-A]pyrimidine-6-carboxylic acid

HRID 1393663ノート

反応式

HRID 1393663 の反応式
[OH-].[Na+].[OH:3][CH2:4][C:5]1[CH:18]=[C:8]2[N:9]=[CH:10][C:11]([C:13]([O:15]CC)=[O:14])=[CH:12][N:7]2[N:6]=1.O>O1CCCC1>[OH:3][CH2:4][C:5]1[CH:18]=[C:8]2[N:9]=[CH:10][C:11]([C:13]([OH:15])=[O:14])=[CH:12][N:7]2[N:6]=1

参加物

5

反応物 3

HCID 962WaterHCID 14798Sodium HydroxideHCID 23091920Ethyl 2-(hydroxymethyl)pyrazolo[1,5-A]pyrimidine-6-carboxylate

生成物 1

HCID 230919552-(Hydroxymethyl)pyrazolo[1,5-A]pyrimidine-6-carboxylic acid収率 66.3%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

5 N Sodium hydroxide solution (0.1 ml) was added to a solution of the thus obtained ethyl 2-hydroxymethylpyrazolo[1,5-a]pyrimidine-6-carboxylate (19 mg) in tetrahydrofuran (1 ml), and stirred for 17 hours at room temperature. After water was added, the reaction mixture was washed with ethyl acetate. The aqueous phase was acidified by 2 N hydrochloric acid, extracted with ethyl acetate and dried over sodium sulfate anhydrous. The resulting product was concentrated under reduced pressure, and the residue was dissolved in hot ethyl acetate and then filtered. The filtrate was concentrated under reduced pressure to give the title compound (11 mg, Y.:65%).

後処理

  1. washthe reaction mixture was washed with ethyl acetate
  2. extractionextracted with ethyl acetate
  3. dry with materialdried over sodium sulfate anhydrous
  4. concentrationThe resulting product was concentrated under reduced pressure
  5. dissolutionthe residue was dissolved in hot ethyl acetate
  6. filtrationfiltered
  7. concentrationThe filtrate was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-29a953d2324e4c91879369d745b8d1ef
出典データセット
uspto-grants-2008_03
特許番号
US07345180B2

反応ノート

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