Ammonium Hydroxide → 4-amino-N-(3,4-dimethyl-phenyl)-3-nitro-benzenesulfonamide

HRID 1514859

반응식

HRID 1514859 반응식
Cl[C:2]1[CH:7]=[CH:6][C:5]([S:8]([NH:11][C:12]2[CH:17]=[CH:16][C:15]([CH3:18])=[C:14]([CH3:19])[CH:13]=2)(=[O:10])=[O:9])=[CH:4][C:3]=1[N+:20]([O-:22])=[O:21].[NH4+:23].[OH-]>O1CCOCC1.O>[NH2:23][C:2]1[CH:7]=[CH:6][C:5]([S:8]([NH:11][C:12]2[CH:17]=[CH:16][C:15]([CH3:18])=[C:14]([CH3:19])[CH:13]=2)(=[O:10])=[O:9])=[CH:4][C:3]=1[N+:20]([O-:22])=[O:21]

참가 물질

5

반응물 2

HCID 14923Ammonium HydroxideHCID 47954984-chloro-N-(3,4-dimethyl-phenyl)-3-nitro-benzenesulfonamide

생성물 1

HCID 669661164-amino-N-(3,4-dimethyl-phenyl)-3-nitro-benzenesulfonamide

시약·촉매·용매 2

HCID 962Water용매HCID 312751,4-Dioxane용매

반응 조건

온도
95 °C

실험 절차

To a suspension of 4-chloro-N-(3,4-dimethyl-phenyl)-3-nitro-benzenesulfonamide (0.22 g) in dioxane (2 mL) was added NH4OH (3 mL). The reaction mixture was heated to 95° C. for 8 h. The mixture was cooled to room temperature, diluted with water, and extracted with CH2Cl2. The extract was dried over Na2SO4 and concentrated in vacuo. Purification by column chromatography (SiO2, 3:1 hexane/EtOAc) afforded 4-amino-N-(3,4-dimethyl-phenyl)-3-nitro-benzenesulfonamide.

후처리

  1. temperatureThe mixture was cooled to room temperature
  2. extractionextracted with CH2Cl2
  3. dry with materialThe extract was dried over Na2SO4
  4. concentrationconcentrated in vacuo
  5. customPurification by column chromatography (SiO2, 3:1 hexane/EtOAc)

출처 및 근거

ORD 기록
ord-b777f18b188341a190f700d440237782
출처 데이터셋
uspto-grants-2012_07
특허 번호
US08222248B2

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