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Aluminium lithium hydride → (4-Benzyl-1-methylpiperazin-2-yl)methanol

HRID 1026428
ノート
印刷プレビュー

反応式

HRID 1026428 の反応式
[CH2:1]([N:8]1[CH2:13][CH2:12][N:11]([C:14](OC(C)(C)C)=O)[CH:10]([C:21](OC)=[O:22])[CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[H-].[Al+3].[Li+].[H-].[H-].[H-]>O1CCCC1>[CH2:1]([N:8]1[CH2:13][CH2:12][N:11]([CH3:14])[CH:10]([CH2:21][OH:22])[CH2:9]1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 21226445Aluminium lithium hydrideHCID 49766299HCID 49766299、化合物

生成物 1

HCID 19777247(4-Benzyl-1-methylpiperazin-2-yl)methanol収率 91.1%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

Compound 111a (1 g, 2.99 mmol) was dissolved in 100 mL of anhydrous tetrahydrofuran and lithium aluminum hydride (342 mg, 8.98 mmol) was added carefully at 0° C. and the mixture was stirred for 30 min. Then, it was refluxed for 3 h and the reaction mixture was poured onto ice portion-wise. It was then filtered and the filtrate was evaporated in vacuo. After addition of 100 mL brine, it was extracted with dichloromethane (100 mL×3). The combined organic layer was dried over Na2SO4, filtered and concentrated to afford 111b as yellow oil (0.6 g, yield 91%)

後処理

  1. temperatureThen, it was refluxed for 3 h
  2. additionthe reaction mixture was poured onto ice portion-wise
  3. filtrationIt was then filtered
  4. customthe filtrate was evaporated in vacuo
  5. additionAfter addition of 100 mL brine, it
  6. extractionwas extracted with dichloromethane (100 mL×3)
  7. dry with materialThe combined organic layer was dried over Na2SO4
  8. filtrationfiltered
  9. concentrationconcentrated

出典と根拠

ORDレコード
ord-599119c079364860a91d1765edf65616
出典データセット
uspto-grants-2014_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08729072B2

反応ノート

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