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Imidazole → 1-[(4-Chlorophenyl)diphenylmethyl]-1H-imidazole

HRID 1580850
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HRID 1580850 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8](Cl)([C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)[C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)=[CH:4][CH:3]=1.[NH:22]1[CH:26]=[CH:25][N:24]=[CH:23]1.C(N(CC)CC)C.Cl.C(N(CC)CC)C>C(#N)C.O.C1C=CC=CC=1>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]([C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)[N:22]2[CH:26]=[CH:25][N:24]=[CH:23]2)=[CH:4][CH:3]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 795ImidazoleHCID 8471TriethylamineHCID 11130Triethylamine hydrochlorideHCID 15629469HCID 15629469, 화합물

생성물 1

HCID 130738771-[(4-Chlorophenyl)diphenylmethyl]-1H-imidazole수율 96.9%

시약·촉매·용매 3

HCID 241Benzene용매
HCID 962
Water
용매
HCID 6342Acetonitrile용매

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온도
50 °C

실험 절차

156.5 g (0.5 mol) of (p-chlorophenyl)-(diphenyl)-methyl chloride and 34 g (0.5 mol) imidazole are dissolved in 500 ml acetonitrile, with stirring, and 51 g (0.5 mol) triethylamine are added, whereupon separation of triethylamine hydrochloride occurs even at room temperature. In order to complete the reaction, heating at 50°C is carried out for three hours. After cooling, 1 liter of benzene is added and the reaction mixture is stirred, then washed salt-free with water. The benzene solution is dried over anhydrous sodium sulfate, filtered and concentrated by evaporation; giving 167 g of crude 1-[(p-chlorophenyl)-(bisphenyl)-methyl]-imidazole, m.p. 125°C. By recrystallization from 200 ml benzene and 100 ml ligroin, 115 g (= 71% of the thoery) of pure 1-[(p-chlorophenyl) (bis-phenyl)-methyl]-imidazole of m.p. 140°C are obtained.

후처리

  1. customoccurs even at room temperature
  2. customthe reaction
  3. temperatureAfter cooling
  4. stirringthe reaction mixture is stirred
  5. dry with materialThe benzene solution is dried over anhydrous sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated by evaporation

출처 및 근거

ORD 기록
ord-85d18aa42c8d4d0d8f0cd0de632a7dec
출처 데이터셋
uspto-grants-1976_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03934022

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