p-Toluenesulfonic acid monohydrate → 1-Methyl-5-(1,3-dioxolan-2-yl)-imidazole

HRID 1936763노트

반응식

HRID 1936763 반응식
[CH3:1][N:2]1[C:6]([CH:7]=[O:8])=[CH:5][N:4]=[CH:3]1.[OH2:9].[C:10]1([CH3:20])C=CC(S(O)(=O)=O)=CC=1>C(O)CO>[CH3:1][N:2]1[C:6]([CH:7]2[O:9][CH2:10][CH2:20][O:8]2)=[CH:5][N:4]=[CH:3]1

참가 물질

4

반응물 2

HCID 521998p-Toluenesulfonic acid monohydrateHCID 5735921-methyl-1H-imidazole-5-carbaldehyde

생성물 1

HCID 226098451-Methyl-5-(1,3-dioxolan-2-yl)-imidazole

시약·촉매·용매 1

HCID 174Ethylene Glycol용매

실험 절차

1-Methyl-5-formyl imidazole (0.64 g) was treated with ethylene glycol (0.3 ml), p-toluenesulphonic acid monohydrate (0.0015 g) and powdered 4A molecular seives under N2 for 18 hours at reflux. Subsequent cooling and filtration was followed by washing of the organic phase with aqueous sodium carbonate solution (2N), drying and concentration to give the title compound; δH (CDCl3) 7.43 (1H,s), 7.12 (1H,s), 5.91 (1H,s), 4.10(4H,m), 3.70(3H,s).

후처리

  1. customfor 18 hours
  2. temperatureat reflux
  3. temperatureSubsequent cooling
  4. filtrationfiltration
  5. washby washing of the organic phase with aqueous sodium carbonate solution (2N)
  6. customdrying
  7. concentrationconcentration

출처 및 근거

ORD 기록
ord-6d03490ed8024c9684f012036f469dc4
출처 데이터셋
uspto-grants-2002_05
특허 번호
US06391874B1

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