Thionyl Chloride → HCID 14802114、化合物

HRID 329722ノート

反応式

HRID 329722 の反応式
[CH3:1][N:2]1[C:7]2[CH:8]=[C:9]([N+:15]([O-:17])=[O:16])[CH:10]=[C:11]([C:12](O)=[O:13])[C:6]=2[O:5][CH2:4][C:3]1=[O:18].S(Cl)([Cl:21])=O>>[CH3:1][N:2]1[C:7]2[CH:8]=[C:9]([N+:15]([O-:17])=[O:16])[CH:10]=[C:11]([C:12]([Cl:21])=[O:13])[C:6]=2[O:5][CH2:4][C:3]1=[O:18]

参加物

3

反応物 2

HCID 24386Thionyl ChlorideHCID 14771561HCID 14771561、化合物

生成物 1

HCID 14802114HCID 14802114、化合物

実験手順

To 99 g of 3,4-dihydro-4-methyl-6-nitro-3-oxo-2H-1,4-benzoxazine-8-carboxylic acid is added portionwise 285 ml of thionyl chloride at room temperature, and the system heated with reflux for about an hour. After the resultant solution is dried under reduced pressure, to the residue is distilled off under reduced pressure. To the residue is added 200 ml of benzene to make the crystals finely particulate. After collecting by filtration, the crystals are washed with benzene and dried to give 103 g of 3,4-dihydro-4-methyl-6-nitro-3-oxo-2H-1,4-benzoxazine-8-carboxylic acid chloride.

後処理

  1. temperaturethe system heated
  2. temperaturewith reflux for about an hour
  3. dry with materialAfter the resultant solution is dried under reduced pressure, to the residue
  4. distillationis distilled off under reduced pressure
  5. additionTo the residue is added 200 ml of benzene
  6. filtrationAfter collecting by filtration
  7. washthe crystals are washed with benzene
  8. customdried

出典と根拠

ORDレコード
ord-43f47df6842b41808fa5e6086efe4779
出典データセット
uspto-grants-1990_01
特許番号
US04892872

反応ノート

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