Imidazole → 1-(diethoxymethyl)-1H-imidazole

HRID 247820

반응식

HRID 247820 반응식
[NH:1]1[CH:5]=[CH:4][N:3]=[CH:2]1.[CH:6](OCC)([O:10][CH2:11][CH3:12])[O:7][CH2:8][CH3:9].C(=O)(O)[O-].[Na+]>C1(C)C=CC(S(O)(=O)=O)=CC=1.C(O)C>[CH2:8]([O:7][CH:6]([O:10][CH2:11][CH3:12])[N:1]1[CH:5]=[CH:4][N:3]=[CH:2]1)[CH3:9]

참가 물질

6

반응물 3

HCID 795ImidazoleHCID 31214Ethyl orthoformateHCID 516892Sodium Bicarbonate

생성물 1

HCID 38495351-(diethoxymethyl)-1H-imidazole수율 68%

시약·촉매·용매 2

HCID 6101p-Toluenesulfonic acid촉매HCID 702Ethanol용매

실험 절차

A mixture of imidazole (15 g, 0.220 mol, 1 eq), triethyl orthoformate (130 g, 146.6 mL, 0.880 mol, 4, eq) and p-toluenesulfonic acid (1.17 g, 0.00616 mol, 0.028 eq) was heated at 145°-175° C. until no more ethanol was distillable from the reaction mixture. The excess orthoformate was removed in vacuo. Solid sodium bicarbonate (1.17 g, 0.011 mol) was added and the residue was vacuum distilled to give the title compound (23.6 g, 68%). b.p. 89°-91° C./0.3 mm Hg.

후처리

  1. customThe excess orthoformate was removed in vacuo
  2. distillationdistilled

출처 및 근거

ORD 기록
ord-6a6261fd93044ce19dd1236baf1910f1
출처 데이터셋
uspto-grants-1993_05
특허 번호
US05208234

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