Iodobenzene → Methyl 3,5-dinitro-4-phenylbenzoate

HRID 1605540노트

반응식

HRID 1605540 반응식
Cl[C:2]1[C:11]([N+:12]([O-:14])=[O:13])=[CH:10][C:5]([C:6]([O:8][CH3:9])=[O:7])=[CH:4][C:3]=1[N+:15]([O-:17])=[O:16].I[C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1>[Cu]>[N+:15]([C:3]1[CH:4]=[C:5]([CH:10]=[C:11]([N+:12]([O-:14])=[O:13])[C:2]=1[C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1)[C:6]([O:8][CH3:9])=[O:7])([O-:17])=[O:16]

참가 물질

4

반응물 2

HCID 11575IodobenzeneHCID 96161Methyl 4-chloro-3,5-dinitrobenzoate

생성물 1

HCID 21546857Methyl 3,5-dinitro-4-phenylbenzoate

시약·촉매·용매 1

HCID 23978Copper촉매

실험 절차

A mixture of methyl 4-chloro-3,5-dinitrobenzoate (60 g), iodobenzene (36 ml) and copper powder (60 g) is stirred at 145°-155° C for 4-5 hours. After cooling, the resulting solids are extracted with three portions of boiling chloroform (each portion 150 ml), and the combined extracts are, after filtration, evaporated in vacuo. After trituration of the residue with methanol (150 ml) followed by recrystallization from 2-methoxyethanol, methyl 3,5-dinitro-4-phenylbenzoate is obtained with a melting point of 147.5°-148° C.

후처리

  1. temperatureAfter cooling
  2. extractionthe resulting solids are extracted with three portions of boiling chloroform (each portion 150 ml), and the combined extracts
  3. filtrationafter filtration
  4. customevaporated in vacuo
  5. customAfter trituration of the residue with methanol (150 ml) followed by recrystallization from 2-methoxyethanol

출처 및 근거

ORD 기록
ord-dc5bb42f2fb24000b6eba0bb2dbf472e
출처 데이터셋
uspto-grants-1976_04
특허 번호
US03950380

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