Methane → 2-Bromo-3-nitrobenzoyl chloride

HRID 1491621

반응식

HRID 1491621 반응식
[Br:1][C:2]1[C:10]([N+:11]([O-:13])=[O:12])=[CH:9][CH:8]=[CH:7][C:3]=1[C:4](O)=[O:5].S(Cl)([Cl:16])=O.C>CC1C=CC=CC=1>[Br:1][C:2]1[C:10]([N+:11]([O-:13])=[O:12])=[CH:9][CH:8]=[CH:7][C:3]=1[C:4]([Cl:16])=[O:5]

참가 물질

5

반응물 3

HCID 297MethaneHCID 24386Thionyl ChlorideHCID 684522-Bromo-3-nitrobenzoic acid

생성물 1

HCID 2229532-Bromo-3-nitrobenzoyl chloride수율 81.7%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

To a stirred suspension of 414 parts of 2-bromo-3-nitrobenzoic acid in 653 parts of methylbenzene there were added 440 parts of thionyl chloride. The whole was refluxed for 6 hours, cooled and left overnight. The reaction mixture was treated with activated charcoal, filtered over diatomaceous earth and evaporated. The residual oil was triturated with 396 parts of hexane (2×). The product was filtered off, washed with hexane and dried, yielding 363 parts (81.7%) of 2-bromo-3-nitrobenzoyl chloride (interm. 3).

후처리

  1. temperatureThe whole was refluxed for 6 hours
  2. temperaturecooled
  3. filtrationfiltered over diatomaceous earth
  4. customevaporated
  5. customThe residual oil was triturated with 396 parts of hexane (2×)
  6. filtrationThe product was filtered off
  7. washwashed with hexane
  8. customdried

출처 및 근거

ORD 기록
ord-dc78b28494bc463ca731b611c6d79bae
출처 데이터셋
uspto-grants-1994_12
특허 번호
US05371079

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