Water → methyl 2-methyl-3-oxo-3,4-dihydro-2H-1,4-benzoxazine-6-carboxylate

HRID 234896ノート

反応式

HRID 234896 の反応式
[NH2:1][C:2]1[CH:7]=[C:6]([C:8]([O:10][CH3:11])=[O:9])[CH:5]=[CH:4][C:3]=1[OH:12].C(=O)([O-])[O-].[K+].[K+].Cl[CH:20]([CH3:24])[C:21](Cl)=[O:22].O>CN(C)C=O.C(OCC)(=O)C>[CH3:11][O:10][C:8]([C:6]1[CH:5]=[CH:4][C:3]2[O:12][CH:20]([CH3:24])[C:21](=[O:22])[NH:1][C:2]=2[CH:7]=1)=[O:9]

参加物

7

反応物 4

HCID 962WaterHCID 10815Methyl 3-amino-4-hydroxybenzoateHCID 11430Potassium CarbonateHCID 1110192-Chloropropionyl chloride

生成物 1

HCID 10656590methyl 2-methyl-3-oxo-3,4-dihydro-2H-1,4-benzoxazine-6-carboxylate収率 71%

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

反応条件

温度
50 °C

実験手順

To a solution of 2-amino-4-methoxycarbonylphenol [Acta Chimica Academiae Scientiarum Hungaricae, 99(1), 49-50 (1979)] (5.0 g) in dimethylformamide (30 ml) were added potassium carbonate (8.3 g) and 2-chloropropionyl chloride (4.0 g) and the mixture was stirred at 50° C. for 2 hours. Water was added to the reaction solution and extraction with ethyl acetate was conducted. The extraction was concentrated and hexane was added thereto to give precipitates, which were taken by filtration and dried to give 6-methoxycarbonyl-2-methyl-3-oxo-3,4-dihydro-2H-1,4-benzoxazine (4.7 g).

後処理

  1. extractionThe extraction
  2. concentrationwas concentrated
  3. additionhexane was added
  4. customto give
  5. customprecipitates
  6. filtrationwhich were taken by filtration
  7. customdried

出典と根拠

ORDレコード
ord-834a2a3c29424ed6bb03e48c07199506
出典データセット
uspto-grants-1997_01
特許番号
US05597820

反応ノート

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