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

HRID 866487

반응식

HRID 866487 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.CS(O)(=O)=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

5

반응물 3

HCID 962WaterHCID 6395Methanesulfonic AcidHCID 595293N-[[(3,5-dichlorophenyl)amino]carbonyl]glycine

생성물 1

HCID 1686913-(3,5-Dichlorophenyl)-2,4-imidazolidinedione수율 95.3%

시약·촉매·용매 1

HCID 7964Chlorobenzene용매

반응 조건

온도
15 °C

실험 절차

To a suspension of 3-(3,5-dichlorophenyl)-ureidoacetic acid (526 g.) in chlorobenzene (2,250 cc.) is added methanesulphonic acid (d = 1.48) (10 cc., representing 0.077 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 (467 g.) melting at 199° C is obtained. Yield: 94%.

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-3c3722fd6f2d44169a5439e24aec2148
출처 데이터셋
uspto-grants-1978_07
특허 번호
US04099008

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