Water → 3-(3,5-Dichlorophenyl)-2,4-imidazolidinedione

HRID 866486

반응식

HRID 866486 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([NH:9][C:10](=[O:16])[NH:11][CH2:12][C:13](O)=[O:14])[CH:5]=[C:6]([Cl:8])[CH:7]=1.S(=O)(=O)(O)O.N(CC(O)=O)C(N)=O.O>ClC1C=CC=CC=1>[Cl:1][C:2]1[CH:3]=[C:4]([N:9]2[C:13](=[O:14])[CH2:12][NH:11][C:10]2=[O:16])[CH:5]=[C:6]([Cl:8])[CH:7]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 1118Sulfuric AcidHCID 10020Hydantoic acidHCID 595293N-[[(3,5-dichlorophenyl)amino]carbonyl]glycine

생성물 1

HCID 1686913-(3,5-Dichlorophenyl)-2,4-imidazolidinedione수율 95.6%

시약·촉매·용매 1

HCID 7964Chlorobenzene용매

반응 조건

온도
15 °C

실험 절차

To a suspension of 3-(3,5-dichlorophenyl)-ureidoacetic acid (813 g.) in chlorobenzene (3,500 cc.) is added concentrated sulphuric acid (d = 1.83) (16 cc.), representing 0.095 mol per mol of ureidoacetic acid. The water formed in the reaction is removed by azeotropic distillation. After 45 minutes' distillation, a limpid solution is obtained. After cooling to about 15° C, the precipitate formed is filtered off and washed on the filter with ethanol (500 cc.) at 10° C. After drying, 3-(3,5-dichlorophenyl)-hydantoin (724 g.) melting at 199° C is obtained. Yield: 95.4%.

후처리

  1. customis removed by azeotropic distillation
  2. distillationAfter 45 minutes' distillation
  3. customa limpid solution is obtained
  4. customthe precipitate formed
  5. filtrationis filtered off
  6. washwashed on the
  7. filtrationfilter with ethanol (500 cc.) at 10° C
  8. customAfter drying

출처 및 근거

ORD 기록
ord-be996351cfeb41cdad920d3b577d1ac0
출처 데이터셋
uspto-grants-1978_07
특허 번호
US04099008

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