Hydrochloric Acid → Methyl 3-(chlorocarbonyl)-5-nitrobenzoate

HRID 1261181ノート

反応式

HRID 1261181 の反応式
[CH3:1][O:2][C:3](=[O:16])[C:4]1[CH:12]=[C:11]([N+:13]([O-:15])=[O:14])[CH:10]=[C:6]([C:7](O)=[O:8])[CH:5]=1.[ClH:17]>S(Cl)(Cl)=O>[CH3:1][O:2][C:3](=[O:16])[C:4]1[CH:12]=[C:11]([N+:13]([O-:15])=[O:14])[CH:10]=[C:6]([C:7]([Cl:17])=[O:8])[CH:5]=1

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 747761,3-Benzenedicarboxylic acid, 5-nitro-, 1-methyl ester

生成物 1

HCID 74774Methyl 3-(chlorocarbonyl)-5-nitrobenzoate

試薬・触媒・溶媒 1

HCID 24386Thionyl Chloride溶媒

実験手順

A suspension of 5-nitro-isophthalic acid mono methyl ester (22.52 g, 100.0 mmol) in thionyl chloride (50 ml) was heated to reflux for 6 hours (until the production of SO2 and HCl-gas ceased). The excess of thionyl chloride was removed under reduced pressure, the residue was dissolved in DCM and the product was precipitated by addition of hexane to give a white solid. Yield: 24.10 g (99%).

後処理

  1. temperaturewas heated
  2. customThe excess of thionyl chloride was removed under reduced pressure
  3. dissolutionthe residue was dissolved in DCM
  4. customthe product was precipitated by addition of hexane
  5. customto give a white solid

出典と根拠

ORDレコード
ord-0fba3e45dacc44129240e3da748448cb
出典データセット
uspto-grants-2013_06
特許番号
US08470860B2

反応ノート

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