N,N-Dimethylaniline → 1,6-dichloro-7-methoxy-4-nitro-9(10H)-acridinone

HRID 280260ノート

反応式

HRID 280260 の反応式
[Cl:1][C:2]1[C:7]([C:8]([OH:10])=O)=[C:6]([NH:11][C:12]2[CH:17]=[CH:16][C:15]([O:18][CH3:19])=[C:14]([Cl:20])[CH:13]=2)[C:5]([N+:21]([O-:23])=[O:22])=[CH:4][CH:3]=1.P(Cl)(Cl)(Cl)=O.CN(C)C1C=CC=CC=1>ClCCCl>[Cl:1][C:2]1[C:7]2[C:8](=[O:10])[C:17]3[C:12](=[CH:13][C:14]([Cl:20])=[C:15]([O:18][CH3:19])[CH:16]=3)[NH:11][C:6]=2[C:5]([N+:21]([O-:23])=[O:22])=[CH:4][CH:3]=1

参加物

5

反応物 3

HCID 949N,N-DimethylanilineHCID 24813Phosphorus oxychlorideHCID 135883476-Chloro-2-[(3-chloro-4-methoxyphenyl)amino]-3-nitrobenzoic acid

生成物 1

HCID 135883311,6-dichloro-7-methoxy-4-nitro-9(10H)-acridinone

試薬・触媒・溶媒 1

HCID 111,2-Dichloroethane溶媒

実験手順

A mixture of 17 g of 6-chloro-2-[(3-chloro-4-methoxyphenyl)amino]-3-nitrobenzoic acid, 35 ml of phosphorus oxychloride, 1 ml of N,N-dimethylaniline and 150 ml 1,2-dichloroethane was heated under reflux for 45 minutes. The resulting solid was collected by filtration from the hot reaction mixture and was washed with chloroform to provide 1,6-dichloro-7-methoxy-4-nitro-9(10H)-acridinone, mp 284°-285° C.

後処理

  1. temperaturewas heated
  2. temperatureunder reflux for 45 minutes
  3. filtrationThe resulting solid was collected by filtration from the hot reaction mixture
  4. washwas washed with chloroform

出典と根拠

ORDレコード
ord-6deb89f2f8274ae29ed35081d8032961
出典データセット
uspto-grants-1986_05
特許番号
US04588730

反応ノート

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