Ammonium Hydroxide → HCID 69654843, 화합물

HRID 1061210노트

반응식

HRID 1061210 반응식
[CH3:1][C:2]([C:4]1[CH:9]=[CH:8][C:7]([Cl:10])=[C:6]([N+:11]([O-])=O)[CH:5]=1)=[O:3].O.O.[Sn](Cl)(Cl)(Cl)Cl.[OH-].[NH4+]>Cl.O>[C:2]([C:4]1[CH:9]=[CH:8][C:7]([Cl:10])=[C:6]([NH:11][C:4]2[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=2)[CH:5]=1)(=[O:3])[CH3:1]

참가 물질

6

반응물 3

HCID 14923Ammonium HydroxideHCID 795964'-Chloro-3'-nitroacetophenoneHCID 85782573Tin tetrachloride dihydrate

생성물 1

HCID 69654843HCID 69654843, 화합물

시약·촉매·용매 2

HCID 313Hydrochloric Acid용매HCID 962Water용매

실험 절차

To a stirred solution of 4-chloro-3-nitroacetophenone (10 g, 50 mmol) in concentracted hydrochloric acid (150 mL) was added tin chloride dihydrate (33.8 g, 150 mmol). The mixture was stirred at room temperature for one day, basified with 28% of ammonium hydroxide and diluted with water (1 L). The aqueous solution was extracted with methylene chloride. The organic phase was dried over MgSO4 and concentrated. Recrystallization from CH2Cl2/hexanes gave the title compound as a yellowish crystal (7.0 g, 83%); 1H NMR (300 MHz, CDCl3) δ 2.55 (s, 3H), 4.19 (brs, 2H), 7.22-7.38 (m, 3H); MS (ES) m/z: 169.8 (MH+, 100%); HRMS Calcd. for C8H9ClNO (MH+): 170.3667. Found: 170.0368.

후처리

  1. extractionThe aqueous solution was extracted with methylene chloride
  2. dry with materialThe organic phase was dried over MgSO4
  3. concentrationconcentrated
  4. customRecrystallization from CH2Cl2/hexanes

출처 및 근거

ORD 기록
ord-57ca89dda8764977b93042e84344e5f9
출처 데이터셋
uspto-grants-2003_02
특허 번호
US06525202B2

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