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

HRID 236939

반응식

HRID 236939 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

HCID 96161Methyl 4-chloro-3,5-dinitrobenzoate수율 89%

시약·촉매·용매 1

HCID 1118Sulfuric Acid용매

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-c33b0a758598405cafca331d6911881a
출처 데이터셋
uspto-grants-1979_06
특허 번호
US04159278

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