Acetic Acid → HCID 12433874, 화합물

HRID 261960

반응식

HRID 261960 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 12433874HCID 12433874, 화합물

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-10440b84c3d940bfab89d4a4ea5e8fa5
출처 데이터셋
uspto-grants-1979_05
특허 번호
US04152441

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