Methyl iodide → Methyl 3-[(methanesulfonyl)(methyl)amino]-5-nitrobenzoate

HRID 1160448노트

반응식

HRID 1160448 반응식
[CH3:1][S:2]([NH:5][C:6]1[CH:7]=[C:8]([CH:13]=[C:14]([N+:16]([O-:18])=[O:17])[CH:15]=1)[C:9]([O:11][CH3:12])=[O:10])(=[O:4])=[O:3].CI.[C:21](=O)([O-])[O-].[K+].[K+]>CC(C)=O>[CH3:21][N:5]([S:2]([CH3:1])(=[O:3])=[O:4])[C:6]1[CH:7]=[C:8]([CH:13]=[C:14]([N+:16]([O-:18])=[O:17])[CH:15]=1)[C:9]([O:11][CH3:12])=[O:10]

참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 57815097Methyl 3-(methylsulfonamido)-5-nitrobenzoate

생성물 1

HCID 57815130Methyl 3-[(methanesulfonyl)(methyl)amino]-5-nitrobenzoate수율 99%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

A mixture of methyl 3-[(methylsulfonyl)amino]-5-nitrobenzoate obtained in Reference Example 88.22 g (30 mmol), methyl iodide 2.0 mL (32 mmol), potassium carbonate 10.4 g (75 mmol) and acetone (250 mL) was stirred at room temperature for 16 hours. The mixture was filtered to remove the precipitates and the solvent was evaporated. To the residue was added water (150 mL) and the mixture was extracted twice with ethyl acetate (100 mL). After drying of the mixture on magnesium sulfate, the solvent was evaporated to give 8.55 g (29.7 mmol) of the title compound (yield: 99%).

후처리

  1. filtrationThe mixture was filtered
  2. customto remove the
  3. customprecipitates
  4. customthe solvent was evaporated
  5. additionTo the residue was added water (150 mL)
  6. extractionthe mixture was extracted twice with ethyl acetate (100 mL)
  7. customAfter drying of the mixture on magnesium sulfate
  8. customthe solvent was evaporated

출처 및 근거

ORD 기록
ord-a2860c02e8c9473eabd8e00f5bc52bf8
출처 데이터셋
uspto-grants-2010_10
특허 번호
US07816387B2

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