Thionyl Chloride → HCID 19804733、化合物

HRID 1682151ノート

反応式

HRID 1682151 の反応式
[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]

参加物

3

反応物 2

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

生成物 1

HCID 19804733HCID 19804733、化合物

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-1215d782a66f4cd1a978e7125a1e7fcf
出典データセット
uspto-grants-1992_12
特許番号
US05175299

反応ノート

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