Ethanone, 2-(2-imidazolidinylidene)-1-phenyl- → 2-(2-Ethoxy-2-phenyl-ethenyl)-2-imidazoline tetrafluoroborate

HRID 66165

反応式

HRID 66165 の反応式
[CH2:1]([O+](CC)CC)[CH3:2].[F:8][B-:9]([F:12])([F:11])[F:10].[NH:13]1[CH2:17][CH2:16][NH:15][C:14]1=[CH:18][C:19]([C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1)=[O:20]>C(Cl)Cl>[CH2:1]([O:20][C:19]([C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1)=[CH:18][C:14]1[NH:13][CH2:17][CH2:16][N:15]=1)[CH3:2].[F:8][B-:9]([F:12])([F:11])[F:10]

参加物

4

反応物 2

HCID 821546Ethanone, 2-(2-imidazolidinylidene)-1-phenyl-HCID 2723982Triethyloxonium tetrafluoroborate

生成物 1

HCID 867362182-(2-Ethoxy-2-phenyl-ethenyl)-2-imidazoline tetrafluoroborate

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

20 g (0.105 mole) of triethyloxonium-tetrafluoroborate is dissolved in 200 ml of methylene chloride. To the solution is added 18.8 g (0.1 mole) of crystalline 2-(2-imidazolidinylidene)-acetophenone [m.p. 211°-212°, see J. Klosa, Arch.Pharmaz. 286, 397 (1953)]. After the slightly exothermic reaction has subsided, the reaction mixture, a clear yellow solution, is stirred for 16 hours at room temperature; it is subsequently concentrated to dryness in the rotary evaporator; and the crystallising residue is suspended in 300 ml of ethyl acetate. The suspension is cooled to 5°, and the crystals are filtered off with suction to obtain 2-(2-ethoxy-2-phenyl-ethenyl)-2-imidazoline-tetrafluoroborate, m.p. 151°-152°. After drying at 60° in vacuo, the product is further employed without additional purification.

後処理

  1. customAfter the slightly exothermic reaction
  2. concentrationit is subsequently concentrated to dryness in the rotary evaporator
  3. temperatureThe suspension is cooled to 5°
  4. filtrationthe crystals are filtered off with suction

出典と根拠

ORDレコード
ord-7949cbad5ce44b3bb410b158ea87f323
出典データセット
uspto-grants-1978_12
特許番号
US04130652

関連ノート

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