Hydrochloric Acid → HCID 20279438、化合物

HRID 1248356ノート

反応式

HRID 1248356 の反応式
[Cl:1][C:2]1[CH:20]=[CH:19][CH:18]=[C:17]([Cl:21])[C:3]=1[C:4]([C:6]1[C:15]([OH:16])=[CH:14][C:9]2[C:10]([C:12]#[N:13])=[CH:11][C:8]=2[CH:7]=1)=[O:5].[OH:22]O.[OH-].[Na+].Cl>C(O)C>[Cl:1][C:2]1[CH:20]=[CH:19][CH:18]=[C:17]([Cl:21])[C:3]=1[C:4]([C:6]1[C:15]([OH:16])=[CH:14][C:9]2[C:10]([C:12]([NH2:13])=[O:22])=[CH:11][C:8]=2[CH:7]=1)=[O:5]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 784Hydrogen PeroxideHCID 14798Sodium HydroxideHCID 20279442HCID 20279442、化合物

生成物 1

HCID 20279438HCID 20279438、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

2 g of 4-(2,6-dichlorobenzoyl)-5-hydroxybenzocyclobutene-1-carbonitrile are dissolved in 50 ml of ethanol, the whole is cooled to 0° and, while stirring at 0°, 10 g of 30% hydrogen peroxide are added dropwise thereto. 1.0 ml of 30% sodium hydroxide solution is then added slowly dropwise thereto and stirring is carried out for 6 hours at room temperature. The whole is neutralised with 6N hydrochloric acid and extracted thoroughly by shaking with 250 ml of dichloromethane. The organic phase is dried over magnesium sulphate and concentrated to dryness by evaporation. After recrystallisation from ether/hexane, 4-(2,6-dichlorobenzoyl)-5-hydroxybenzocyclobutene-1-carboxamide is obtained having a melting point of 174°-175°.

後処理

  1. temperaturethe whole is cooled to 0°
  2. stirringstirring
  3. extractionextracted thoroughly
  4. stirringby shaking with 250 ml of dichloromethane
  5. dry with materialThe organic phase is dried over magnesium sulphate
  6. concentrationconcentrated to dryness by evaporation
  7. customAfter recrystallisation from ether/hexane

出典と根拠

ORDレコード
ord-ff5ef970487546e4aae6be86a6dd32f9
出典データセット
uspto-grants-1985_06
特許番号
US04523030

反応ノート

読み込み中…