Hydrochloric Acid → Ethyl 3-acetylamino-2-nitrobenzoate

HRID 1276887노트

반응식

HRID 1276887 반응식
[C:1](Cl)(=[O:3])[CH3:2].[NH2:5][C:6]1[C:7]([N+:17]([O-:19])=[O:18])=[C:8]([CH:14]=[CH:15][CH:16]=1)[C:9]([O:11][CH2:12][CH3:13])=[O:10].Cl>CN(C)C1C=CC=CC=1>[C:1]([NH:5][C:6]1[C:7]([N+:17]([O-:19])=[O:18])=[C:8]([CH:14]=[CH:15][CH:16]=1)[C:9]([O:11][CH2:12][CH3:13])=[O:10])(=[O:3])[CH3:2]

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 6367Acetyl chlorideHCID 18315537Ethyl 3-amino-2-nitrobenzoate

생성물 1

HCID 18315582Ethyl 3-acetylamino-2-nitrobenzoate

시약·촉매·용매 1

HCID 949N,N-Dimethylaniline용매

실험 절차

Acetyl chloride (13 ml) was added dropwise to a solution of 2.98 g of ethyl 3-amino-2-nitrobenzoate and 20 ml of N,N-dimethylaniline in an ice bath. The mixture was stirred at room temperature for 48 hours. The reaction solution was acidified with 10% hydrochloric acid, and was extracted twice with ethyl acetate. The organic layer was washed three times with water. The solvent was distilled off under reduced pressure, and the resulting residue was crystallized with hexane. The crystals were separated through filtration, washed with hexane, and dried to give 3.30 g of ethyl 3-acetylamino-2-nitrobenzoate.

후처리

  1. extractionwas extracted twice with ethyl acetate
  2. washThe organic layer was washed three times with water
  3. distillationThe solvent was distilled off under reduced pressure
  4. customthe resulting residue was crystallized with hexane
  5. customThe crystals were separated through filtration
  6. washwashed with hexane
  7. customdried

출처 및 근거

ORD 기록
ord-6e003abc9eed4e3f9be2b2a64d666ae6
출처 데이터셋
uspto-grants-2000_12
특허 번호
US06166219

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