Phosgene → HCID 12861465, 화합물

HRID 614515노트

반응식

HRID 614515 반응식
[CH3:1][C:2]([C:4]1[CH:9]=[C:8]([Cl:10])[C:7]([NH2:11])=[C:6]([Cl:12])[CH:5]=1)=[O:3].[C:13](Cl)(Cl)=[O:14]>C1(C)C=CC=CC=1>[C:2]([C:4]1[CH:5]=[C:6]([Cl:12])[C:7]([N:11]=[C:13]=[O:14])=[C:8]([Cl:10])[CH:9]=1)(=[O:3])[CH3:1]

참가 물질

4

반응물 2

HCID 6371PhosgeneHCID 6048121-(4-Amino-3,5-dichlorophenyl)ethan-1-one

생성물 1

HCID 12861465HCID 12861465, 화합물

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

A mixture of 5 g. of 4-amino-3,5-dichloroacetophenone, 5 ml. of phosgene, and 30 ml. of toluene was heated to 150° C. for 24 hours in a sealed tube. The reaction mixture was cooled and concentrated under reduced pressure to provide crude 4-acetyl-2,6-dichlorophenyl isocyanate. The crude product was dissolved in 100 ml. of toluene and then dry dimethylamine was passed through the solution for one hour at room temperature. The reaction mixture was concentrated under reduced pressure and the residue formed was recrystallized from a mixture of benzene and n-hexane to provide 2.58 g. of 3,5-dichloro-4-N,N-dimethylcarbamoylaminoacetophenone having a melting point of 138°-140° C.

후처리

  1. additionA mixture of 5 g
  2. temperatureThe reaction mixture was cooled
  3. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-0bf87f46d6cb49108b6450c92ae04f85
출처 데이터셋
uspto-grants-1979_03
특허 번호
US04145363

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