Methanol → 2-Hydroxy-5-methylsulfamoyl-benzoic acid methyl ester

HRID 1352272ノート

反応式

HRID 1352272 の反応式
[OH:1][C:2]1[CH:10]=[CH:9][C:8]([S:11](=[O:15])(=[O:14])[NH:12][CH3:13])=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].[CH:16]1N=CN(C(N2C=NC=C2)=O)C=1.CO>C1COCC1>[CH3:16][O:5][C:4](=[O:6])[C:3]1[CH:7]=[C:8]([S:11](=[O:15])(=[O:14])[NH:12][CH3:13])[CH:9]=[CH:10][C:2]=1[OH:1]

参加物

5

反応物 3

HCID 887MethanolHCID 682631,1'-CarbonyldiimidazoleHCID 144900612-Hydroxy-5-methylsulfamoyl-benzoic acid

生成物 1

HCID 230467632-Hydroxy-5-methylsulfamoyl-benzoic acid methyl ester

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
70 °C

実験手順

To 77 mmol 2-hydroxy-5-methylsulfamoyl-benzoic acid in 300 ml THF was added 85 mmol CDI and the mixture heated at 70° C. for 1 h. 770 mmol methanol was then added and the mixture was heated at 70° C. for 16 h. The mixture was then cooled to room temperature and concentrated in vacuo. The residue was chromatographed on silica gel (eluant: ethyl acetate/heptane/dichloromethane 45:45:10) to afford the title compound. MS (m/e): 244.1 ([M−H]−, 100%)

後処理

  1. temperaturethe mixture was heated at 70° C. for 16 h
  2. temperatureThe mixture was then cooled to room temperature
  3. concentrationconcentrated in vacuo
  4. customThe residue was chromatographed on silica gel (eluant: ethyl acetate/heptane/dichloromethane 45:45:10)

出典と根拠

ORDレコード
ord-f8482bdb7bd04b1e9f1c57aabaf9e74f
出典データセット
uspto-grants-2007_05
特許番号
US07220744B2

反応ノート

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