Methane → 2-Bromo-3-nitrobenzoyl chloride

HRID 1532442

反応式

HRID 1532442 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

HCID 2229532-Bromo-3-nitrobenzoyl chloride収率 81.7%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-5cbc86a98c5f4d2d92a316ff95d84f06
出典データセット
uspto-grants-2001_03
特許番号
US06201119B1

関連ノート

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