Water → 4-(7-(Butyl)-3-mesityl-2,5-dimethylpyrazolo[1,5-a]pyrimidin-yl)-1-butanol

HRID 966004ノート

反応式

HRID 966004 の反応式
[H-].C([Al+]CC(C)C)C(C)C.[CH2:11]([C:15]1[N:20]2[N:21]=[C:22]([CH3:33])[C:23]([C:24]3[C:29]([CH3:30])=[CH:28][C:27]([CH3:31])=[CH:26][C:25]=3[CH3:32])=[C:19]2[N:18]=[C:17]([CH3:34])[C:16]=1[CH2:35][CH2:36][CH2:37][C:38](OCC)=[O:39])[CH2:12][CH2:13][CH3:14].C(OCC)(=O)C.O>CCCCCC.O1CCCC1>[CH2:11]([C:15]1[N:20]2[N:21]=[C:22]([CH3:33])[C:23]([C:24]3[C:25]([CH3:32])=[CH:26][C:27]([CH3:31])=[CH:28][C:29]=3[CH3:30])=[C:19]2[N:18]=[C:17]([CH3:34])[C:16]=1[CH2:35][CH2:36][CH2:37][CH2:38][OH:39])[CH2:12][CH2:13][CH3:14]

参加物

7

反応物 4

HCID 962WaterHCID 8857Ethyl AcetateHCID 21225700DiisobutylaluminumhydrideHCID 22249666Ethyl 4-(7-(butyl)-3-mesityl-2,5-dimethylpyrazolo[1,5-a]pyrimidin-6-yl)butanoate

生成物 1

HCID 222495124-(7-(Butyl)-3-mesityl-2,5-dimethylpyrazolo[1,5-a]pyrimidin-yl)-1-butanol収率 114.5%

試薬・触媒・溶媒 2

HCID 8028Tetrahydrofuran溶媒HCID 8058Hexane溶媒

実験手順

A 1.0M solution of diisobutylaluminium hydride in hexane was added dropwise into a solution of ethyl 4-(7-(butyl)-3-mesityl-2,5-dimethylpyrazolo[1,5-a]pyrimidin-6-yl)butanoate (320 mg, 0.71 mmol) in tetrahydrofuran (10 mL) under nitrogen stream, followed by stirring for 30 minutes. After Celite was added, the mixture was treated by adding ethyl acetate and water dropwise, and the insoluble matters were filtered off. The solution was extracted with ethyl acetate, dried over anhydrous magnesium sulfate and evaporated, to give the title compound (320 mg) as a brown oil.

後処理

  1. additionAfter Celite was added
  2. additionthe mixture was treated
  3. filtrationthe insoluble matters were filtered off
  4. extractionThe solution was extracted with ethyl acetate
  5. dry with materialdried over anhydrous magnesium sulfate
  6. customevaporated

出典と根拠

ORDレコード
ord-aa07ee062bf94fddb895329db10a0145
出典データセット
uspto-grants-2005_10
特許番号
US06951865B2

反応ノート

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