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Sodium Acetate → Ethyl pyrazolo[1,5-a]pyrimidine-5-carboxylate

HRID 1443839
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HRID 1443839 반응식
[CH2:1]([O:3][C:4]([C:6]1[CH:11]=[C:10](Cl)[N:9]2[N:13]=[CH:14][CH:15]=[C:8]2[N:7]=1)=[O:5])[CH3:2].C([O-])(=O)C.[Na+]>[Pd].C(OCC)(=O)C.C(O)C>[CH2:1]([O:3][C:4]([C:6]1[CH:11]=[CH:10][N:9]2[N:13]=[CH:14][CH:15]=[C:8]2[N:7]=1)=[O:5])[CH3:2]
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참가 물질

5

반응물 2

HCID 517045Sodium AcetateHCID 12366074Ethyl 7-chloropyrazolo[1,5-a]pyrimidine-5-carboxylate

생성물 1

HCID 49763022Ethyl pyrazolo[1,5-a]pyrimidine-5-carboxylate수율 78%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 21584252Ethanol ethylacetate용매

실험 절차

A suspension of 7-chloro-pyrazolo-[1,5-a]-pyrimidine-5-carboxylic acid ethyl ester (15.0 g), sodium acetate (6.54 g), and 10% palladium on carbon (665 mg) in ethyl acetate-ethanol (1-1.50 mL) was stirred under a hydrogen atmosphere. After the completion of the reaction, the reactant was filtered, and concentrated in vacuo. The residue was dissolved in ethyl acetate, washed with water, aqueous baking soda, and brine, dried with sodium sulfate, and concentrated in vacuo. The yellow residue was recrystallized to yield a light yellow needle crystal (9.9 g, 78%). mp:114-115° C.

후처리

  1. customAfter the completion of the reaction
  2. filtrationthe reactant was filtered
  3. concentrationconcentrated in vacuo
  4. dissolutionThe residue was dissolved in ethyl acetate
  5. washwashed with water, aqueous baking soda, and brine
  6. dry with materialdried with sodium sulfate
  7. concentrationconcentrated in vacuo
  8. customThe yellow residue was recrystallized

출처 및 근거

ORD 기록
ord-0092383681d845dcba430ac49717792e
출처 데이터셋
uspto-grants-2010_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07662826B2

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