Methanol → Methyl 4-chloro-3,5-dinitrobenzoate

HRID 236939

反応式

HRID 236939 の反応式
[Cl:1][C:2]1[C:10]([N+:11]([O-:13])=[O:12])=[CH:9][C:5]([C:6]([OH:8])=[O:7])=[CH:4][C:3]=1[N+:14]([O-:16])=[O:15].[CH3:17]O>S(=O)(=O)(O)O>[Cl:1][C:2]1[C:3]([N+:14]([O-:16])=[O:15])=[CH:4][C:5]([C:6]([O:8][CH3:17])=[O:7])=[CH:9][C:10]=1[N+:11]([O-:13])=[O:12]

参加物

4

反応物 2

HCID 887MethanolHCID 83774-Chloro-3,5-dinitrobenzoic acid

生成物 1

HCID 96161Methyl 4-chloro-3,5-dinitrobenzoate収率 89%

試薬・触媒・溶媒 1

HCID 1118Sulfuric Acid溶媒

実験手順

4-Chloro-3,5-dinitrobenzoic acid (25.0 gm.) is dissolved in a cooled solution of methanol (125 ml.) and concentrated sulfuric acid (3.0 ml.). The reaction mixture is allowed to warm to room temperature and then heated to reflux for 18 hours. The product precipitated as light yellow needles on cooling, which are collected by filtration and washed with 15 ml. of methanol (24.0 gm., m.p. 102°-104.5°). Recrystallization from methanol gives light yellow needles (23.6 g., m.p. 104- 105.5). 89% yield).

後処理

  1. temperatureheated
  2. temperatureto reflux for 18 hours
  3. customThe product precipitated as light yellow needles
  4. temperatureon cooling
  5. filtrationwhich are collected by filtration
  6. washwashed with 15 ml
  7. customRecrystallization from methanol
  8. customgives light yellow needles (23.6 g., m.p. 104- 105.5)

出典と根拠

ORDレコード
ord-c33b0a758598405cafca331d6911881a
出典データセット
uspto-grants-1979_06
特許番号
US04159278

関連ノート

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