Triethylamine → 2-Butyramido-4-nitrophenyl trifluoromethanesulfonate

HRID 40117

反応式

HRID 40117 の反応式
[OH:1][C:2]1[CH:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[CH:4][C:3]=1[NH:11][C:12](=[O:16])[CH2:13][CH2:14][CH3:15].CCN(CC)CC.[O:24](S(C(F)(F)F)(=O)=O)[S:25]([C:28]([F:31])([F:30])[F:29])(=O)=[O:26]>C(Cl)Cl>[F:29][C:28]([F:31])([F:30])[S:25]([O:1][C:2]1[CH:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[CH:4][C:3]=1[NH:11][C:12](=[O:16])[CH2:13][CH2:14][CH3:15])(=[O:26])=[O:24]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 67749Trifluoromethanesulfonic anhydrideHCID 3599768N-(2-hydroxy-5-nitrophenyl)butanamide2 回

生成物 1

HCID 112912342-Butyramido-4-nitrophenyl trifluoromethanesulfonate

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

To a solution of N-(2-hydroxy-5-nitrophenyl)butyramide (Compound 117, 1.75 g, 7.8 mmol) in CH2Cl2 (40 ml) at 0° C. was added Et3N (1.4 ml, 10.1 mmol) and Tf2O (1.7 ml, 10.2 mmol). After 10 min, the reaction was diluted with CH2Cl2, washed with H2O and brine, dried over Na2SO4, and concentrated in vacuo. The residue was purified by chromatography on silica gel (0→25% EtOAc-hexanes) to yield the title compound.

後処理

  1. washwashed with H2O and brine
  2. dry with materialdried over Na2SO4
  3. concentrationconcentrated in vacuo
  4. customThe residue was purified by chromatography on silica gel (0→25% EtOAc-hexanes)

出典と根拠

ORDレコード
ord-da175815e55247df81ca8bc698266e3a
出典データセット
uspto-grants-2013_09
特許番号
US08524917B2

関連ノート

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