Phosgene → HCID 12861465、化合物

HRID 614515ノート

反応式

HRID 614515 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

HCID 12861465HCID 12861465、化合物

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-0bf87f46d6cb49108b6450c92ae04f85
出典データセット
uspto-grants-1979_03
特許番号
US04145363

反応ノート

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