Potassium Iodide → HCID 21321305, 화합물

HRID 261971

반응식

HRID 261971 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]([C:15]2[CH:20]=[CH:19][C:18]([Cl:21])=[CH:17][CH:16]=2)([C:10]2[NH:11][CH:12]=[CH:13][N:14]=2)[OH:9])=[CH:4][CH:3]=1.[C:22]1(C(O)=C([N+]([O-])=O)C=C([N+]([O-])=O)C=1)[N+]([O-])=O.[I-].[K+].[OH-].[Na+].CI>C(#N)C>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]([C:15]2[CH:20]=[CH:19][C:18]([Cl:21])=[CH:17][CH:16]=2)([C:10]2[N:14]([CH3:22])[CH:13]=[CH:12][N:11]=2)[OH:9])=[CH:6][CH:7]=1

참가 물질

7

반응물 5

HCID 4875Potassium IodideHCID 6328Methyl iodideHCID 6954Picric AcidHCID 14798Sodium HydroxideHCID 12433870Bis-(4-chloro-phenyl)-(1H-imidazol-2-yl)-methanol

생성물 1

HCID 21321305HCID 21321305, 화합물

시약·촉매·용매 1

HCID 6342Acetonitrile용매2회

실험 절차

To a suspension of 9.6 g (0.030 mol) of α,α-bis(p-chlorophenyl)imidazole-2-methanol (prepared according to Example III) in 100 ml. of acetonitrile, 500 mg of picric acid, 300 mg of potassium iodide and 1.45 g (0.036 mol) of sodium hydroxide were added at 60° C. The reaction mixture was stirred for one hour and then 4.7 g (0.033 mol) of methyl iodide in 25 ml. of acetonitrile were added dropwise at 55° C. The mixture was refluxed for four hours, the solvent was distilled off and the residue was extracted with a mixture of water and diethyl ether. The solid matter was filtered off and the ethereal phase was dried over sodium sulphate and concentrated. Diethyl ether was added to the residue and the solid matter was filtered off. The two portions of solid material were combined and twice crystallised from isopropyl alcohol and twice from toluene and rewashed with petroleum ether (boiling range 60°-80° C.). α,α-Bis(p-chlorophenyl)-1-methylimidazole-2-methanol was obtained. Melting point 190°-191° C.

후처리

  1. temperatureThe mixture was refluxed for four hours
  2. distillationthe solvent was distilled off
  3. extractionthe residue was extracted with a mixture of water and diethyl ether
  4. filtrationThe solid matter was filtered off
  5. dry with materialthe ethereal phase was dried over sodium sulphate
  6. concentrationconcentrated
  7. additionDiethyl ether was added to the residue
  8. filtrationthe solid matter was filtered off
  9. customtwice crystallised from isopropyl alcohol and twice from toluene

출처 및 근거

ORD 기록
ord-fa1e8f200d2b431ba484ee83dd61595a
출처 데이터셋
uspto-grants-1979_05
특허 번호
US04152441

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