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Dimethylamine → HCID 12952964、化合物

HRID 2286237
ノート
印刷プレビュー

反応式

HRID 2286237 の反応式
[ClH:1].[Cl:2][CH2:3][CH2:4][CH:5]1[CH2:9][N:8]([CH3:10])[C:7](=[NH:11])[N:6]1[CH3:12].[CH3:13][NH:14][CH3:15].C[OH:17]>>[OH2:17].[ClH:2].[ClH:1].[NH:11]=[C:7]1[N:6]([CH3:12])[CH:5]([CH2:4][CH2:3][N:14]([CH3:15])[CH3:13])[CH2:9][N:8]1[CH3:10]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 3

HCID 674DimethylamineHCID 887MethanolHCID 20542259HCID 20542259、化合物

生成物 1

HCID 12952964HCID 12952964、化合物収率 26%

実験手順

To 10.0 g (0.047 mole) of 4-(2-chloroethyl)-2-imino-1,3-dimethylimidazolidine hydrochloride was added 6.8 g (0.15 mole) of dimethylamine in 175 ml of methanol. The mixture was heated in a steel bomb at 100° C. for 15 hours. After concentrating in vacuo, the residue was partitioned between a dilute sodium carbonate solution and chloroform. The organic layer was dried (Na2SO4), filtered, and concentrated in vacuo. The residue was dissolved in ethyl acetate and treated with ethereal HCl. The hydrochloride was recrystallized from ethanol twice, and weighed 3.2 g (26% yield); m.p. 210°-212° C.

後処理

  1. concentration
After concentrating in vacuo
  • customthe residue was partitioned between a dilute sodium carbonate solution and chloroform
  • dry with materialThe organic layer was dried (Na2SO4)
  • filtrationfiltered
  • concentrationconcentrated in vacuo
  • dissolutionThe residue was dissolved in ethyl acetate
  • additiontreated with ethereal HCl
  • customThe hydrochloride was recrystallized from ethanol twice
  • 出典と根拠

    ORDレコード
    ord-bed42c60be7f4640a6f36472818164b8
    出典データセット
    uspto-grants-1982_04
    DOI
    10.6084/m9.figshare.5104873.v1
    特許番号
    US04327107

    反応ノート

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