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

HRID 1160448ノート

反応式

HRID 1160448 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-a2860c02e8c9473eabd8e00f5bc52bf8
出典データセット
uspto-grants-2010_10
特許番号
US07816387B2

反応ノート

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