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

HRID 383148

反応式

HRID 383148 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-7cff57209b0a4774829073d5d421076a
出典データセット
uspto-grants-2001_10
特許番号
US06310095B1

関連ノート

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