Water → HCID 178498045, 화합물

HRID 2164622

반응식

HRID 2164622 반응식
[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]

참가 물질

6

반응물 4

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

생성물 1

HCID 178498045HCID 178498045, 화합물수율 75.2%

시약·촉매·용매 1

HCID 24813Phosphorus oxychloride용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-026a6d3952fa4328a8677a98144acf0c
출처 데이터셋
uspto-grants-1985_03
특허 번호
US04505926

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