Trityl chloride → Bifonazole

HRID 1111658

반응식

HRID 1111658 반응식
[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

참가 물질

5

반응물 3

HCID 6456Trityl chlorideHCID 1110064-(Chlorophenylmethyl)-1,1'-biphenyl2회HCID 14420972TMS-Imidazole

생성물 1

HCID 2378Bifonazole수율 52.1%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-5bffc8abda5f4c0ba78b60f58d66befa
출처 데이터셋
uspto-grants-1978_10
특허 번호
US04118487

연결된 노트

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