Hydrochloric Acid → N-(3-tert-Butyl-2-hydroxy-5-methoxyphenyl)-N'-phenylurea

HRID 1457570노트

반응식

HRID 1457570 반응식
Cl.[C:2]1([NH:8][C:9](=[O:27])[NH:10][C:11]2[CH:20]=[C:19]([O:21][CH3:22])[CH:18]=[C:17]([C:23]([CH3:26])([CH3:25])[CH3:24])[C:12]=2[O:13]COC)[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1>CO>[C:2]1([NH:8][C:9](=[O:27])[NH:10][C:11]2[CH:20]=[C:19]([O:21][CH3:22])[CH:18]=[C:17]([C:23]([CH3:24])([CH3:26])[CH3:25])[C:12]=2[OH:13])[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 22099424[2-(3-Phenylureido)-4-methoxy-6-tert-butylphenoxy]methoxymethane

생성물 1

HCID 22099432N-(3-tert-Butyl-2-hydroxy-5-methoxyphenyl)-N'-phenylurea수율 83%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

Conc. hydrochloric acid (1.5 ml) was added to 30 ml of a methanol solution containing 2.2 g of [2-(3-phenyl-ureido)-4-methoxy-6-tert-butylphenoxy]methoxymethane and the mixture was stirred at room temperature for 1.5 hours. The solvent was removed under reduced pressure and the residue was extracted with ethyl acetate. The extract was washed and dried, and the solvent was removed under reduced pressure. Hexane was added to the residue and the resulting crystals were collected by filtration and recrystallized from a mixed solution of ethyl acetate and hexane to give 1.6 g of 2-(3-phenylureido)-4-methoxy-6-tert-butylphenol (yield: 83%, melting point: 147°-149° C., IR: 3400, 3350, 1670 cm-1).

후처리

  1. customThe solvent was removed under reduced pressure
  2. extractionthe residue was extracted with ethyl acetate
  3. washThe extract was washed
  4. customdried
  5. customthe solvent was removed under reduced pressure
  6. additionHexane was added to the residue
  7. filtrationthe resulting crystals were collected by filtration
  8. customrecrystallized from a mixed solution of ethyl acetate and hexane

출처 및 근거

ORD 기록
ord-61103e6bc4f34402a8feff31b23650e2
출처 데이터셋
uspto-grants-1998_12
특허 번호
US05849732

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