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Ethyl Acetate → N,N-Dimethyl-N′-[3-[[(methylamino)carbonyl]oxy]phenyl]thiourea

HRID 1076287
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인쇄 미리보기

반응식

HRID 1076287 반응식
[CH3:1][N:2]([CH3:13])[C:3]([NH:5][C:6]1[CH:11]=[CH:10][CH:9]=[C:8]([OH:12])[CH:7]=1)=[S:4].C(OCC)(=O)C.[CH3:20][N:21]=[C:22]=[O:23]>CCCCCC>[CH3:1][N:2]([CH3:13])[C:3]([NH:5][C:6]1[CH:11]=[CH:10][CH:9]=[C:8]([O:12][C:22](=[O:23])[NH:21][CH3:20])[CH:7]=1)=[S:4]
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참가 물질

5

반응물 3

HCID 8857Ethyl AcetateHCID 12228Methyl IsocyanateHCID 5368133Thiourea, N'-(3-hydroxyphenyl)-N,N-dimethyl-

생성물 1

HCID 21493114N,N-Dimethyl-N′-[3-[[(methylamino)carbonyl]oxy]phenyl]thiourea

시약·촉매·용매 1

HCID 8058Hexane용매

반응 조건

온도
20 °C

실험 절차

1,1-dimethyl-3-(meta-methylcarbamoyloxyphenyl)-2-thiourea is prepared by charging to a suitable equipped reaction vessel about 32.7 parts by weight of 1,1-dimethyl-3-(meta-hydroxyphenyl)-2-thiourea, about 100 parts by weight of ethyl acetate, about 12 parts by weight of methyl isocyanate and about 1 part by weight triethylamino, refluxing for about 1 hour with stirring, diluting the resulting slurry with about 100 parts by weight of hexane, cooling to about 20°C., recovering the precipitate from the remainder by filtration, washing the recovered solid with ethyl acetate and hexane and air drying.

후처리

  1. customa suitable equipped
  2. customrecovering the precipitate from the remainder
  3. filtrationby filtration
  4. washwashing the recovered solid with ethyl acetate and hexane and air
  5. customdrying

출처 및 근거

ORD 기록
ord-82214dc61492436b9804a644c655d3ba
출처 데이터셋
uspto-grants-1976_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03956384

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