Acetic Acid → HCID 12433874、化合物

HRID 261960

反応式

HRID 261960 の反応式
[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[CH:4][C:3]=1[C:9]([C:19]1[CH:24]=[CH:23][C:22]([Cl:25])=[CH:21][C:20]=1[Cl:26])([C:11]1[N:12](COC)[CH:13]=[CH:14][N:15]=1)[OH:10].C(O)(=O)C.Cl>O>[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[CH:4][C:3]=1[C:9]([C:19]1[CH:24]=[CH:23][C:22]([Cl:25])=[CH:21][C:20]=1[Cl:26])([C:11]1[NH:15][CH:14]=[CH:13][N:12]=1)[OH:10]

参加物

5

反応物 3

HCID 176Acetic AcidHCID 313Hydrochloric AcidHCID 12433909alpha,alpha-Bis(2,4-dichlorophenyl)-1-(methoxymethyl)imidazole-2-methanol

生成物 1

HCID 12433874HCID 12433874、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A solution of 10 g (0.023 mol) of α,α-bis(2,4-dichlorophenyl)-1-(methoxymethyl)imidazole-2-methanol in 150 ml. of glacial acetic acid, 15 ml. of concentrated hydrochloric acid and 15 ml. of water was refluxed for two hours and then concentrated. The residue was dissolved in a small amount of a mixture of ethanol and 2N hydrochloric acid and the solution was extracted with diethyl ether. The extract was dried over sodium sulphate and the ether was distilled off. Diethyl ether and petroleum ether (boiling range 60°-80° C.) were added, the solid substance was filtered off and twice crystallised from isopropyl alcohol with a little ethanol. α,α-Bis(2,4-dichlorophenyl)imidazole-2-methanol was obtained. Melting point 193° C.

後処理

  1. concentrationconcentrated
  2. dissolutionThe residue was dissolved in a small amount of a mixture of ethanol and 2N hydrochloric acid
  3. extractionthe solution was extracted with diethyl ether
  4. dry with materialThe extract was dried over sodium sulphate
  5. distillationthe ether was distilled off
  6. additionDiethyl ether and petroleum ether (boiling range 60°-80° C.) were added
  7. filtrationthe solid substance was filtered off
  8. customtwice crystallised from isopropyl alcohol with a little ethanol

出典と根拠

ORDレコード
ord-10440b84c3d940bfab89d4a4ea5e8fa5
出典データセット
uspto-grants-1979_05
特許番号
US04152441

関連ノート

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