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

HRID 1452616
ノート
印刷プレビュー

反応式

HRID 1452616 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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).

このページの内容参加物実験手順後処理出典と根拠反応ノート

後処理

  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)

出典と根拠

ORDレコード
ord-d0ee2f71c925443fb96d97d43f472a63
出典データセット
uspto-grants-2009_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07473694B2

反応ノート

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