Sodium Hydroxide → HCID 14349631、化合物

HRID 329940

反応式

HRID 329940 の反応式
[OH-].[Na+].[OH:3][C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[C:10]([N:12]1[CH:16]=[CH:15][N:14]=[CH:13]1)=[CH2:11].Cl[CH2:18][C:19]([CH3:23])=[C:20]([CH3:22])[CH3:21]>CO>[CH3:18][C:19](=[C:20]([CH3:22])[CH3:21])[CH2:23][O:3][C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[C:10]([N:12]1[CH:16]=[CH:15][N:14]=[CH:13]1)=[CH2:11]

参加物

5

反応物 3

HCID 14798Sodium HydroxideHCID 28055362-[1-(1H-imidazol-1-yl)vinyl]phenolHCID 122407322-Butene, 1-chloro-2,3-dimethyl-

生成物 1

HCID 14349631HCID 14349631、化合物収率 63%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

9.2 g (0.23 mol) of sodium hydroxide are added to a mixture of 39.1 g (0.21 mol) of 1-[1-(2-hydroxyphenyl)-vinyl]-imidazole and 200 ml of methanol at room temperature, with stirring. When the addition has ended, the mixture is stirred at 50° C. for a further 30 minutes and is then concentrated under reduced pressure by stripping off the solvent. The solid residue which remains is taken up in 200 ml of dimethylformamide. 24.9 g (0.21 mol) of 1-chloro-2,3-dimethyl-but-2-ene are added to the solution formed at a temperature of 25° C., with stirring. The reaction mixture is stirred at 20° C. for a further 12 hours and then worked up by being concentrated by stripping off the diluent. The residue obtained is chromatographed over silica gel. 35.5 g (63% of theory) of 1-[1-(2-(2,3-dimethyl-but-2-en-1-yl-oxy)phenyl)-vinyl]-imidazole in the form of an oil are obtained in this manner.

後処理

  1. additionWhen the addition
  2. stirringthe mixture is stirred at 50° C. for a further 30 minutes
  3. concentrationis then concentrated under reduced pressure
  4. customformed at a temperature of 25° C.
  5. stirringwith stirring
  6. stirringThe reaction mixture is stirred at 20° C. for a further 12 hours
  7. concentrationby being concentrated
  8. customThe residue obtained
  9. customis chromatographed over silica gel

出典と根拠

ORDレコード
ord-c0ab425eb82c45c8ab1134fb16dd1688
出典データセット
uspto-grants-1990_01
特許番号
US04894381

関連ノート

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