Butyl iodide → N--t-Butoxycarbonyl-N-butyl-O-benzylhydroxylamine

HRID 383148

반응식

HRID 383148 반응식
[C:1]([O:5][C:6]([NH:8][O:9][CH2:10][C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1)=[O:7])([CH3:4])([CH3:3])[CH3:2].[H-].[Na+].I[CH2:20][CH2:21][CH2:22][CH3:23]>C1COCC1>[C:1]([O:5][C:6]([N:8]([CH2:20][CH2:21][CH2:22][CH3:23])[O:9][CH2:10][C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1)=[O:7])([CH3:4])([CH3:2])[CH3:3]

참가 물질

5

반응물 3

HCID 10962Butyl iodideHCID 24758Sodium hydrideHCID 736159Tert-butyl N-(benzyloxy)carbamate

생성물 1

HCID 53942485N--t-Butoxycarbonyl-N-butyl-O-benzylhydroxylamine

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a stirred solution at 0° C. of N--t-Butoxycarbonyl-O-benzylhydroxylamine, prepared as in Example 1175A, in anhydrous THF was added portionwise a 60% dispersion of sodium hydride (1.2 equiv.) in mineral oil. Mixture stirred 30 minutes ar 0° C., and then, 1-iodobutane (1.2 equiv.) was added dropwise. Reaction stirred one hour at 0° C., and than, overnight at room temperature. Reaction concentrated in vacuo. Residue taken up in EtOAc and washed with water, 1.0M NaHCO3, 1N H3PO4, and brine. Organic layer dried with Na2SO4, filtered, and evaporated.

후처리

  1. customar 0° C.
  2. customReaction
  3. stirringstirred one hour at 0° C.
  4. customovernight
  5. customat room temperature
  6. customReaction
  7. concentrationconcentrated in vacuo
  8. washwashed with water, 1.0M NaHCO3, 1N H3PO4, and brine
  9. dry with materialOrganic layer dried with Na2SO4
  10. filtrationfiltered
  11. customevaporated

출처 및 근거

ORD 기록
ord-7cff57209b0a4774829073d5d421076a
출처 데이터셋
uspto-grants-2001_10
특허 번호
US06310095B1

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