Hydrochloric Acid → 1-(5-amino-2-chlorophenyl)ethanone

HRID 1742006노트

반응식

HRID 1742006 반응식
[CH3:1][C:2]([C:4]1[CH:9]=[C:8]([N+:10]([O-])=O)[CH:7]=[CH:6][C:5]=1[Cl:13])=[O:3].C(O)C.Cl.C(=O)([O-])[O-].[K+].[K+]>O.[Fe]>[CH3:1][C:2]([C:4]1[CH:9]=[C:8]([NH2:10])[CH:7]=[CH:6][C:5]=1[Cl:13])=[O:3]

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 702EthanolHCID 11430Potassium CarbonateHCID 899961-(2-Chloro-5-nitrophenyl)ethan-1-one

생성물 1

HCID 15019111-(5-amino-2-chlorophenyl)ethanone

시약·촉매·용매 2

HCID 23925Iron촉매HCID 962Water용매2회

실험 절차

5 g of solid 2-chloro-5-nitroacetophenone (see J. Am. Chem. Soc. 76, 5482 (1952)) are introduced in portions and with stirring at 65° C. to a mixture of 5.6 g of iron powder, 40 ml of ethanol, 9 ml of water and 1 ml of concentrated hydrochloric acid. Stirring of the reaction mixture is continued for 1 hour at 70° C. The mixture is allowed to cool to room temperature and then diluted with 300 ml of water, and a pH of 9 is established by adding 2N potassium carbonate solution. The mixture is filtered with suction through Celite, and the residue is washed with 200 ml of ethyl acetate. The filtrate is transferred to a separating funnel, and the aqueous phase is discarded. The organic phase is washed with saturated sodium chloride solution, dried over sodium sulfate and concentrated.

후처리

  1. filtrationThe mixture is filtered with suction through Celite
  2. washthe residue is washed with 200 ml of ethyl acetate
  3. customThe filtrate is transferred to a separating funnel
  4. washThe organic phase is washed with saturated sodium chloride solution
  5. dry with materialdried over sodium sulfate
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-feb17e5f2234486982ff99672b9803eb
출처 데이터셋
uspto-grants-1994_08
특허 번호
US05336663

반응 노트

불러오는 중…