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

HRID 275837노트

반응식

HRID 275837 반응식
[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]

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-42ee668c66c54ecca5a8a6bf9f2152ae
출처 데이터셋
uspto-grants-2002_03
특허 번호
US06352982B1

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