Diethyl Ether → tert-butyl N-[(2S)-4-methyl-1-oxopentan-2-yl]carbamate

HRID 22450

反応式

HRID 22450 の反応式
[H-].[Al+3].[Li+].[H-].[H-].[H-].CON(C)[C:10](=[O:24])[C@H:11]([CH2:20][CH:21]([CH3:23])[CH3:22])[NH:12][C:13]([O:15][C:16]([CH3:19])([CH3:18])[CH3:17])=[O:14].S([O-])(O)(=O)=O.[K+].CCOCC>O>[C:16]([O:15][C:13]([NH:12][C@H:11]([CH:10]=[O:24])[CH2:20][CH:21]([CH3:22])[CH3:23])=[O:14])([CH3:18])([CH3:19])[CH3:17]

参加物

6

反応物 4

HCID 3283Diethyl EtherHCID 516920Potassium bisulfateHCID 11119284(S)-N-methyl-N-methoxy-2-(tert-butoxycarbonylamino)-4-methylpentanamideHCID 21226445Aluminium lithium hydride

生成物 1

HCID 104275tert-butyl N-[(2S)-4-methyl-1-oxopentan-2-yl]carbamate

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

Lithium aluminum hydride (2.5 equiv.) is added to a stirred solution of compound (7). Reduction is complete within 15-20 minutes. The mixture is hydrolyzed with a solution of potassium hydrogen sulfate in water. Ether is added and the aqueous phase is separated and extracted. The organic phases are combined, washed with 1N HCl saturated sodium hydrogen carbonate and saturated sodium chloride, and dried with magnesium sulfate. The solvent is evaporated to leave the desired product

後処理

  1. customthe aqueous phase is separated
  2. extractionextracted
  3. washwashed with 1N HCl saturated sodium hydrogen carbonate and saturated sodium chloride
  4. dry with materialdried with magnesium sulfate
  5. customThe solvent is evaporated

出典と根拠

ORDレコード
ord-c05cdbbfbba14f20a453eb4c70efeaa1
出典データセット
uspto-grants-1995_06
特許番号
US05428019

関連ノート

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