Triethylamine → 1-[4-(4-Ethoxyphenoxy)benzyl]-2-methylbenzimidazole

HRID 65089

반응식

HRID 65089 반응식
[CH3:1][C:2]1[NH:3][C:4]2[CH:10]=[CH:9][CH:8]=[CH:7][C:5]=2[N:6]=1.C(N(CC)CC)C.[CH2:18]([O:20][C:21]1[CH:35]=[CH:34][C:24]([O:25][C:26]2[CH:33]=[CH:32][C:29]([CH2:30]Cl)=[CH:28][CH:27]=2)=[CH:23][CH:22]=1)[CH3:19]>C1(C)C=CC=CC=1>[CH2:18]([O:20][C:21]1[CH:35]=[CH:34][C:24]([O:25][C:26]2[CH:33]=[CH:32][C:29]([CH2:30][N:3]3[C:4]4[CH:10]=[CH:9][CH:8]=[CH:7][C:5]=4[N:6]=[C:2]3[CH3:1])=[CH:28][CH:27]=2)=[CH:23][CH:22]=1)[CH3:19]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 119842-MethylbenzimidazoleHCID 137303804-(4-Ethoxyphenoxy)benzyl chloride

생성물 1

HCID 135634041-[4-(4-Ethoxyphenoxy)benzyl]-2-methylbenzimidazole수율 88.1%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

A mixture of toluene (20 ml), 2-methylbenzimidazole (0.55 g, 4.2 mmole), triethylamine (0.42 g, 4.2 mmole) and 4-(4-ethoxyphenoxy)benzyl chloride (1.00 g, 3.8 mmole) was heated under reflux for 5 hours and then cooled to room temperature. The resultant mixture was washed with water, dried over anhydrous sodium sulfate and distilled under reduced pressure to remove toluene. The residue was purified by silica gel column chromatography to give 1-[4-(4-ethoxyphenoxy)benzyl]-2-methylbenzimidazole (1.20 g) as colorless liquid. nD26.0 1.5984.

후처리

  1. temperaturewas heated
  2. temperatureunder reflux for 5 hours
  3. washThe resultant mixture was washed with water
  4. dry with materialdried over anhydrous sodium sulfate
  5. distillationdistilled under reduced pressure
  6. customto remove toluene
  7. customThe residue was purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-4d3582a376fb4abda8b517ac664f2d3e
출처 데이터셋
uspto-grants-1986_09
특허 번호
US04612323

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