Butanedione → 4-Isopropoxymethyl-2-(p-methoxyphenyl)-5-methylimidazole hydrochloride

HRID 839125

반응식

HRID 839125 반응식
[ClH:1].[CH3:2][O:3][C:4]1[CH:12]=[CH:11][C:7]([C:8]([NH2:10])=[NH:9])=[CH:6][CH:5]=1.[C:13]([C:16]([CH3:18])=O)([CH3:15])=O>C(O)(C)C>[ClH:1].[CH:4]([O:3][CH2:15][C:13]1[N:9]=[C:8]([C:7]2[CH:11]=[CH:12][C:4]([O:3][CH3:2])=[CH:5][CH:6]=2)[NH:10][C:16]=1[CH3:18])([CH3:12])[CH3:5]

참가 물질

4

반응물 2

HCID 650ButanedioneHCID 123262194-Methoxybenzamidine Hydrochloride

생성물 1

HCID 203258814-Isopropoxymethyl-2-(p-methoxyphenyl)-5-methylimidazole hydrochloride수율 161.9%

시약·촉매·용매 1

HCID 3776Isopropanol용매

실험 절차

To a solution of 38.4 g (0.206 mole) of p-methoxy-benzamidine hydrochloride in 1 liter of refluxing isopropyl alcohol is added 25 g (0.25 mole) of biacetyl. The mixture is stirred and refluxed for 72 hours. The solvent is removed to dryness under reduced pressure and the solid residue taken up in fresh hot isopropyl alcohol. Ether is added and, on chilling, pale yellow crystals form which are collected to give about 49.5 g (81% yield) of 4-isopropoxymethyl-2-(p-methoxyphenyl)-5-methylimidazole hydrochloride as very pale yellow crystals, m.p. 149°-150° C (dec.). Recrystallization twice from isopropyl alcohol-ether with charcoaling gives the product as white crystals, m.p. 149°-150° C (dec.).

후처리

  1. temperaturerefluxed for 72 hours
  2. customThe solvent is removed to dryness under reduced pressure
  3. additionEther is added
  4. temperatureon chilling
  5. custompale yellow crystals form which are collected

출처 및 근거

ORD 기록
ord-b69325bec56f42c09d77d025d7214a05
출처 데이터셋
uspto-grants-1978_06
특허 번호
US04093811

연결된 노트

불러오는 중…