Trityl chloride → Bifonazole

HRID 1111658

反応式

HRID 1111658 の反応式
[C:1]1([C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)[CH:6]=[CH:5][C:4]([CH:7]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)Cl)=[CH:3][CH:2]=1.C1(C(C2C=CC=CC=2)(C2C=CC=CC=2)Cl)C=CC=CC=1.C[Si]([C:45]1[NH:46][CH:47]=[CH:48][N:49]=1)(C)C>C(#N)C>[C:1]1([C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)[CH:6]=[CH:5][C:4]([CH:7]([N:46]2[CH:47]=[CH:48][N:49]=[CH:45]2)[C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)=[CH:3][CH:2]=1

参加物

5

反応物 3

HCID 6456Trityl chlorideHCID 1110064-(Chlorophenylmethyl)-1,1'-biphenyl2 回HCID 14420972TMS-Imidazole

生成物 1

HCID 2378Bifonazole収率 52.1%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

167 g (0.6 mol) of biphenyl-4-yl-phenyl-chloromethane [alternatively named as diphenyl-phenyl-chloromethane or as α-(biphenyl-4-yl)benzyl chloride] and 92 g (0.66 mol) of trimethylsilylimidazole, dissolved in 500 ml of acetonitrile, are heated under reflux for 15 hours. After distilling off the solvent, the crystalline residue is purified by recrystallization from ethyl acetate. 97 g (52% of theory) of (biphenyl-4-yl)-imidazol-1-yl-phenylmethane of melting point 142° C. are obtained.

後処理

  1. temperatureare heated
  2. temperatureunder reflux for 15 hours
  3. distillationAfter distilling off the solvent
  4. customthe crystalline residue is purified by recrystallization from ethyl acetate

出典と根拠

ORDレコード
ord-5bffc8abda5f4c0ba78b60f58d66befa
出典データセット
uspto-grants-1978_10
特許番号
US04118487

関連ノート

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