Water → N-methyl-N-methyloxy-2-benzyloxycarbonylamino-5-isobutyloxybenzamide

HRID 275837ノート

反応式

HRID 275837 の反応式
[CH3:1][N:2]([O:23][CH3:24])[C:3](=[O:22])[C:4]1[CH:9]=[C:8]([OH:10])[CH:7]=[CH:6][C:5]=1[NH:11][C:12]([O:14][CH2:15][C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1)=[O:13].[CH:25](I)([CH3:27])[CH3:26].[C:29](=O)([O-])[O-].[K+].[K+].O>CN(C)C=O>[CH3:1][N:2]([O:23][CH3:24])[C:3](=[O:22])[C:4]1[CH:9]=[C:8]([O:10][CH2:26][CH:25]([CH3:27])[CH3:29])[CH:7]=[CH:6][C:5]=1[NH:11][C:12]([O:14][CH2:15][C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1)=[O:13]

参加物

6

反応物 4

HCID 962WaterHCID 6362Isopropyl iodideHCID 11430Potassium CarbonateHCID 18315375N-methyl-N-methyloxy-2-benzyloxycarbonylamino-5-hydroxybenzamide

生成物 1

HCID 18315337N-methyl-N-methyloxy-2-benzyloxycarbonylamino-5-isobutyloxybenzamide

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A solution of N-methyl-N-methyloxy-2-benzyloxycarbonylamino-5-hydroxybenzamide (3.0 g), isopropyl iodide (2.2 g) and potassium carbonate (2.0 g) in N,N-dimethylformamide (20 ml) was stirred for 15 hours at 70° C. To the reaction mixture was added water, which was subjected to extraction with ethyl acetate (80 ml). The organic layer was washed with water and dried over anhydrous sodium sulfate. The solvent was distilled off, and the residue was purified by means of a silica gel column chromatography to give N-methyl-N-methyloxy-2-benzyloxycarbonylamino-5-isobutyloxybenzamide.as an orange oily product (1.0 g).

後処理

  1. extractionwas subjected to extraction with ethyl acetate (80 ml)
  2. washThe organic layer was washed with water
  3. dry with materialdried over anhydrous sodium sulfate
  4. distillationThe solvent was distilled off
  5. customthe residue was purified by means of a silica gel column chromatography

出典と根拠

ORDレコード
ord-42ee668c66c54ecca5a8a6bf9f2152ae
出典データセット
uspto-grants-2002_03
特許番号
US06352982B1

反応ノート

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