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

HRID 22450

반응식

HRID 22450 반응식
[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]

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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

후처리

  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

출처 및 근거

ORD 기록
ord-c05cdbbfbba14f20a453eb4c70efeaa1
출처 데이터셋
uspto-grants-1995_06
특허 번호
US05428019

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