Water → HCID 178498045、化合物

HRID 2164622

反応式

HRID 2164622 の反応式
[CH3:1][O:2][C:3](=[O:13])[C:4]1[CH:9]=[C:8]([Cl:10])[C:7]([NH2:11])=[C:6]([Cl:12])[CH:5]=1.[C:14]([N:17]1[CH2:21][CH2:20][NH:19][C:18]1=O)(=[O:16])[CH3:15].O.[OH-].[Na+]>P(Cl)(Cl)(Cl)=O>[C:14]([N:17]1[CH2:21][CH2:20][NH:19][C:18]1=[N:11][C:7]1[C:6]([Cl:12])=[CH:5][C:4]([C:3]([O:2][CH3:1])=[O:13])=[CH:9][C:8]=1[Cl:10])(=[O:16])[CH3:15]

参加物

6

反応物 4

HCID 962WaterHCID 14798Sodium HydroxideHCID 79350N-AcetylimidazolidinoneHCID 604808Methyl 4-amino-3,5-dichlorobenzoate

生成物 1

HCID 178498045HCID 178498045、化合物収率 75.2%

試薬・触媒・溶媒 1

HCID 24813Phosphorus oxychloride溶媒2 回

実験手順

Methyl-4-amino-3,5-dichlorobenzoate (16.8 g, 31 mmole), 1-acetyl-2-imidazolidone (4.3 g, 33.5 mmole) in phosphoryl chloride (44 ml) were stirred at 50° C. for 3 days. After cooling the phosphoryl chloride was evaporated to give an oily residue. Iced water was added to the residue which was then basified with aqueous sodium hydroxide. The mixture was extracted with methylene chloride which was then washed with water, dried (magnesium sulphate) and evaporated to give a creamy solid. This solid was recrystallised from toluene to give the title compound (7.7 g) mp 188°-189° C.

後処理

  1. customwas evaporated
  2. customto give an oily residue
  3. extractionThe mixture was extracted with methylene chloride which
  4. washwas then washed with water
  5. dry with materialdried (magnesium sulphate)
  6. customevaporated
  7. customto give a creamy solid
  8. customThis solid was recrystallised from toluene

出典と根拠

ORDレコード
ord-026a6d3952fa4328a8677a98144acf0c
出典データセット
uspto-grants-1985_03
特許番号
US04505926

関連ノート

読み込み中…