Azobisisobutyronitrile → 4-(Difluoromethoxy)benzyl Bromide

HRID 1995673ノート

反応式

HRID 1995673 の反応式
[F:1][CH:2]([F:11])[O:3][C:4]1[CH:9]=[CH:8][C:7]([CH3:10])=[CH:6][CH:5]=1.[Br:12]N1C(=O)CCC1=O.N(C(C)(C)C#N)=NC(C)(C)C#N>C(Cl)(Cl)(Cl)Cl>[F:1][CH:2]([F:11])[O:3][C:4]1[CH:9]=[CH:8][C:7]([CH2:10][Br:12])=[CH:6][CH:5]=1

参加物

5

反応物 3

HCID 6547AzobisisobutyronitrileHCID 67184N-bromobutanimideHCID 74104alpha,alpha-Difluoro-p-methylanisole

生成物 1

HCID 27370014-(Difluoromethoxy)benzyl Bromide収率 62.6%

試薬・触媒・溶媒 1

HCID 5943Carbon Tetrachloride溶媒

実験手順

270 g of 4-difluoromethoxytoluene in 800 ml of CCl4 were initially introduced and 300 g N-bromo-succinimide were added. After adding a pinch of azobisisobutyronitrile, the mixture was heated to the reflux temperature. After 8 hours, it was cooled, the insoluble succinimide was filtered off and the residue on the filter was washed with CCl4. The carbon tetrachloride was distilled off from the reaction solution and the crude product was purified by fractional distillation. 250 g of 4-difluoromethoxy-benzyl bromide were obtained. Boiling point=82°-5° C./0.4 mm Hg; nD20 =1.5200.

後処理

  1. temperaturethe mixture was heated to the reflux temperature
  2. temperatureit was cooled
  3. filtrationthe insoluble succinimide was filtered off
  4. washthe residue on the filter was washed with CCl4
  5. distillationThe carbon tetrachloride was distilled off from the reaction solution
  6. distillationthe crude product was purified by fractional distillation

出典と根拠

ORDレコード
ord-9b6ebbc0c3ee42a69c80b52d37d69a4c
出典データセット
uspto-grants-1983_09
特許番号
US04405639

反応ノート

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