p-Anisoyl chloride → HCID 18174608, 화합물

HRID 427656노트

반응식

HRID 427656 반응식
[NH2:1][C:2]1[C:7]([NH2:8])=[CH:6][CH:5]=[CH:4][C:3]=1[OH:9].[OH-:10].[Na+].[CH3:12][O:13][C:14]1[CH:22]=[CH:21][C:17]([C:18](Cl)=[O:19])=[CH:16][CH:15]=1>C(Cl)Cl>[CH3:12][O:13][C:14]1[CH:22]=[CH:21][C:17]([C:18]([O:10][O:9][C:3]2[CH:4]=[CH:5][CH:6]=[C:7]([NH:8][C:18](=[O:19])[C:17]3[CH:21]=[CH:22][C:14]([O:13][CH3:12])=[CH:15][CH:16]=3)[C:2]=2[NH:1][C:18](=[O:19])[C:17]2[CH:21]=[CH:22][C:14]([O:13][CH3:12])=[CH:15][CH:16]=2)=[O:19])=[CH:16][CH:15]=1

참가 물질

5

반응물 3

HCID 7477p-Anisoyl chlorideHCID 14798Sodium HydroxideHCID 5799372,3-Diaminophenol

생성물 1

HCID 18174608HCID 18174608, 화합물수율 74%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

2,3-Diaminophenol (2.48g, 20 mmol) was dissolved in methylene chloride (200 mL) and the solution was cooled to ice-water bath temperature. Aqueous 5 N sodium hydroxide solution (126 mL) was added followed by 4-methoxybenzoyl chloride (8.6 mL, 63 mmol). The mixture was allowed to warm to room temperature and stirred for 18 h. The organic layer was separated and washed with dilute aqueous sodium hydroxide solution, dilute aqueous hydrochloric acid, and saturated aqueous sodium chloride solution. The organic layer was dried (sodium sulfate), filtered, and concentrated in vacuo to give 7.75 g (74%) of the title compound as a brown foam. This material was used without further purification.

후처리

  1. temperaturethe solution was cooled to ice-water bath temperature
  2. customThe organic layer was separated
  3. washwashed with dilute aqueous sodium hydroxide solution, dilute aqueous hydrochloric acid, and saturated aqueous sodium chloride solution
  4. dry with materialThe organic layer was dried (sodium sulfate)
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-ef2793f9aad8472da56d5ec58903f1a0
출처 데이터셋
uspto-grants-2001_11
특허 번호
US06313122B1

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