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Ammonium Chloride → 2-(5,7-Dichloropyrazolo[1,5-a]pyrimidin-6-yl)ethanol

HRID 1452616
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HRID 1452616 반응식
[Cl:1][C:2]1[C:7]([CH2:8][CH:9]=[O:10])=[C:6]([Cl:11])[N:5]2[N:12]=[CH:13][CH:14]=[C:4]2[N:3]=1.[BH4-].[Na+].[Cl-].[NH4+]>CO>[Cl:1][C:2]1[C:7]([CH2:8][CH2:9][OH:10])=[C:6]([Cl:11])[N:5]2[N:12]=[CH:13][CH:14]=[C:4]2[N:3]=1
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참가 물질

5

반응물 3

HCID 25517Ammonium ChlorideHCID 4311764Sodium borohydrideHCID 866137832-(5,7-Dichloropyrazolo[1,5-a]pyrimidin-6-yl)acetaldehyde

생성물 1

HCID 575268292-(5,7-Dichloropyrazolo[1,5-a]pyrimidin-6-yl)ethanol수율 146.1%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

The above aldehyde (1.82 mmol) was dissolved in methanol (27 mL), and sodium borohydride (302 mg, 7.98 mmol) was added to this solution with ice-cooling. After this mixture was stirred for 30 min, aqueous ammonium chloride was added here. The resultant mixture was extracted with ethyl acetate, and the organic layer was washed with brine and dried over sodium sulfate. After the sodium sulfate was filtered off, the solvent was distilled off, and the residue was purified with column chromatography (15% ethyl acetate-hexane) to obtain the title compound (617 mg).

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후처리

  1. temperaturecooling
  2. extractionThe resultant mixture was extracted with ethyl acetate
  3. washthe organic layer was washed with brine
  4. dry with materialdried over sodium sulfate
  5. filtrationAfter the sodium sulfate was filtered off
  6. distillationthe solvent was distilled off
  7. customthe residue was purified with column chromatography (15% ethyl acetate-hexane)

출처 및 근거

ORD 기록
ord-d0ee2f71c925443fb96d97d43f472a63
출처 데이터셋
uspto-grants-2009_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07473694B2

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