Tetrahydrofuran → HCID 85317206、化合物

HRID 1657192ノート

反応式

HRID 1657192 の反応式
[Cl:1][C:2]1[CH:13]=[CH:12][C:5]([C:6]([NH:10][CH3:11])=[CH:7][C:8]#[N:9])=[CH:4][CH:3]=1.[Br:14]Br.O1CCCC1>C(Cl)(Cl)(Cl)Cl>[Br:14][C:7](=[C:6]([NH:10][CH3:11])[C:5]1[CH:4]=[CH:3][C:2]([Cl:1])=[CH:13][CH:12]=1)[C:8]#[N:9]

参加物

5

反応物 3

HCID 8028TetrahydrofuranHCID 24408Bromine2 回HCID 67753963HCID 67753963、化合物

生成物 1

HCID 85317206HCID 85317206、化合物収率 69%

試薬・触媒・溶媒 1

HCID 5943Carbon Tetrachloride溶媒2 回

反応条件

温度
70 °C

実験手順

A solution of p-chloro-β-(methylamino)cinnamonitrile (19.3 g, 0.1 mol) in carbon tetrachloride at 70° C. is treated dropwise with a solution of bromine (16.8 g, 0.105 mol) in carbon tetrachloride over a 30-40 minute period (tetrahydrofuran is added as needed during the bromine addition to aid dissolution of the reaction mixture). The reaction mixture is stirred for 30 minutes at 70° C., cooled to room temperature and concentrated to give a yellow crystalline precipitate. The mixture is filtered, the filter cake is washed with carbon tetrachloride and dried to give the title product as a yellow solid, 18.8 g (69% yield), mp 178.0°-178.5° C., identified by IR, NMR and mass spectral analyses.

後処理

  1. additionis added
  2. dissolutiondissolution of the reaction mixture)
  3. temperaturecooled to room temperature
  4. concentrationconcentrated
  5. customto give a yellow crystalline precipitate
  6. filtrationThe mixture is filtered
  7. washthe filter cake is washed with carbon tetrachloride
  8. customdried

出典と根拠

ORDレコード
ord-1011f82c72434ea684181eb3fe02a6e7
出典データセット
uspto-grants-1993_10
特許番号
US05256796

反応ノート

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