Hydrochloric Acid → HCID 20279438, 화합물

HRID 1248356노트

반응식

HRID 1248356 반응식
[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]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 784Hydrogen PeroxideHCID 14798Sodium HydroxideHCID 20279442HCID 20279442, 화합물

생성물 1

HCID 20279438HCID 20279438, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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°.

후처리

  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

출처 및 근거

ORD 기록
ord-ff5ef970487546e4aae6be86a6dd32f9
출처 데이터셋
uspto-grants-1985_06
특허 번호
US04523030

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