Hydrochloric Acid → Ethyl 3-acetylamino-2-nitrobenzoate

HRID 276027ノート

反応式

HRID 276027 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

HCID 18315582Ethyl 3-acetylamino-2-nitrobenzoate

試薬・触媒・溶媒 1

HCID 949N,N-Dimethylaniline溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-7a01beb7110244ddb1150a9f6048d994
出典データセット
uspto-grants-2002_03
特許番号
US06352985B1

反応ノート

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