1,3-Dimethyl-2-imidazolidinone → 1,3-Dimethyl-2-diphenylmethyliminoimidazolidine

HRID 46639

反応式

HRID 46639 の反応式
[CH3:1][N:2]1[CH2:6][CH2:5][N:4]([CH3:7])[C:3]1=O.[CH:9]([NH2:22])([C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1)[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1.[OH-].[Na+]>C(Cl)Cl>[CH3:1][N:2]1[CH2:6][CH2:5][N:4]([CH3:7])[C:3]1=[N:22][CH:9]([C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1)[C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1

参加物

5

反応物 3

HCID 66611,3-Dimethyl-2-imidazolidinoneHCID 7036BenzhydrylamineHCID 14798Sodium Hydroxide

生成物 1

HCID 125034181,3-Dimethyl-2-diphenylmethyliminoimidazolidine

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

To 3.79 grams (0.027 mole) of boron trifluoride etherate in 3 milliliters of anhydrous ether under dry argon, is added as rapidly as possible while maintaining control of the reaction, 1.8 gram (0.02 mole) of epichlorohydrin in 7 milliliters of dry ether. After about 3 hours, the crystals of triethyloxonium fluoborate which are formed are separated and washed with fresh dry ether under dry argon. The crystals are then dissolved in dry methylene chloride (5 ml.) and a solution of 2.28 grams (0.02 mole) of 1,3-dimethyl-2-imidazolidinone in 25 milliliters of dry methylene chloride is added. After stirring at room temperature for about 3 hours, 3.66 gram (0.02 mole) of benzhydrylamine in 5 milliliters of methylene chloride is added. The resulting mixture is allowed to stir overnight at room temperature. Treatment of the reaction mixture with excess cold (0° C.) 20% NaOH, shaking, and separation of the organic layer gives a solution of the free base. This solution is dried over anhydrous potassium carbonate, filtered and the solvent is vaporized in vacuo to afford the 1,3-dimethyl-2-diphenylmethyliminoimidazolidine product.

後処理

  1. customare separated
  2. washwashed with fresh dry ether under dry argon
  3. dissolutionThe crystals are then dissolved in dry methylene chloride (5 ml.)
  4. stirringto stir overnight at room temperature
  5. customseparation of the organic layer
  6. customgives a solution of the free base
  7. dry with materialThis solution is dried over anhydrous potassium carbonate
  8. filtrationfiltered

出典と根拠

ORDレコード
ord-00fd6391401b42e9bb00c6cfd759d940
出典データセット
uspto-grants-1979_11
特許番号
US04174401

関連ノート

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