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Aluminium lithium hydride → Tert-butyl 4-(1-hydroxy-2-methylpropan-2-yl)piperazine-1-carboxylate

HRID 888926
ノート
印刷プレビュー

反応式

HRID 888926 の反応式
[H-].[Al+3].[Li+].[H-].[H-].[H-].[C:7]([O:11][C:12]([N:14]1[CH2:19][CH2:18][N:17]([C:20]([C:23](OCC)=[O:24])([CH3:22])[CH3:21])[CH2:16][CH2:15]1)=[O:13])([CH3:10])([CH3:9])[CH3:8]>O1CCCC1>[C:7]([O:11][C:12]([N:14]1[CH2:15][CH2:16][N:17]([C:20]([CH3:22])([CH3:21])[CH2:23][OH:24])[CH2:18][CH2:19]1)=[O:13])([CH3:10])([CH3:9])[CH3:8]
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 57420344HCID 57420344、化合物

生成物 1

HCID 57420345Tert-butyl 4-(1-hydroxy-2-methylpropan-2-yl)piperazine-1-carboxylate収率 39.1%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a suspension of lithium aluminium hydride powder (0.324 g) in anhydrous tetrahydrofuran (30 mL) at 0° C. under argon was added 4-(1-ethoxycarbonyl-1-methyl-ethyl)-piperazin-1-carboxylic acid tert-butyl ester (1.28 g). The reaction mixture was allowed to warm to room temperature and stirred for 2 hours, then quenched with saturated aqueous ammonium chloride (10 mL). The reaction mixture was partitioned between water and dichloromethane and the combined organic layers washed with brine and dried (MgSO4). The solution was evaporated to give 4-(2-hydroxy-1,1-dimethyl-ethyl)-piperazin-1-carboxylic acid tert-butyl ester (0.43 g).

後処理

  1. customquenched with saturated aqueous ammonium chloride (10 mL)
  2. customThe reaction mixture was partitioned between water and dichloromethane
  3. washthe combined organic layers washed with brine
  4. dry with materialdried (MgSO4)
  5. customThe solution was evaporated

出典と根拠

ORDレコード
ord-9e52ce89e97f4fe79edf685e842a807e
出典データセット
uspto-grants-2012_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08252792B2

反応ノート

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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