Thionyl Chloride → HCID 19804733, 화합물

HRID 1682151노트

반응식

HRID 1682151 반응식
[Cl:1][C:2]1[C:10]([N+:11]([O-:13])=[O:12])=[C:9]([Cl:14])[CH:8]=[CH:7][C:3]=1[C:4](O)=[O:5].S(Cl)([Cl:17])=O>>[Cl:1][C:2]1[C:10]([N+:11]([O-:13])=[O:12])=[C:9]([Cl:14])[CH:8]=[CH:7][C:3]=1[C:4]([Cl:17])=[O:5]

참가 물질

3

반응물 2

HCID 24386Thionyl ChlorideHCID 190232292,4-Dichloro-3-nitrobenzoic acid

생성물 1

HCID 19804733HCID 19804733, 화합물

실험 절차

23.0 g of 2,4-dichloro-3-nitrobenzoic acid and 150 ml of thionyl chloride were refluxed for 6 hours under heating. Then, thionyl chloride was distilled off to obtain crude 2,4-dichloro-3-nitrobenzoyl chloride. 200 ml of methanol was added to the crude compound and refluxed under heating. Methanol was distilled off, and then ethyl acetate was added thereto to obtain an ethyl acetate solution. The solution was washed sequentially with a 5% sodium hydroxide aqueous solution, diluted hydrochloric acid and water. After drying, the solvent was distilled off to obtain 21.8 g of the desired product. Melting point: 72°-74° C.

후처리

  1. temperatureunder heating
  2. distillationThen, thionyl chloride was distilled off

출처 및 근거

ORD 기록
ord-1215d782a66f4cd1a978e7125a1e7fcf
출처 데이터셋
uspto-grants-1992_12
특허 번호
US05175299

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