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

HRID 1393663노트

반응식

HRID 1393663 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-29a953d2324e4c91879369d745b8d1ef
출처 데이터셋
uspto-grants-2008_03
특허 번호
US07345180B2

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