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Cyclohexylamine → HCID 525618、化合物

HRID 223318
ノート
印刷プレビュー

反応式

HRID 223318 の反応式
[Cl-].Cl[C:3](=[N+:10]([CH3:12])[CH3:11])[C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1.[CH:13]1([NH2:19])[CH2:18][CH2:17][CH2:16][CH2:15][CH2:14]1>C(Cl)Cl>[CH:13]1([N:19]=[C:3]([C:4]2[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=2)[N:10]([CH3:12])[CH3:11])[CH2:18][CH2:17][CH2:16][CH2:15][CH2:14]1
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 2

HCID 7965CyclohexylamineHCID 10954662Methanaminium, N-(chlorophenylmethylene)-N-methyl-, chloride

生成物 1

HCID 525618HCID 525618、化合物収率 49%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

To the solution of (α-chlorobenzylidene)dimethylammonium chloride in methylenechloride described in Example 1, there was added dropwise, a solution of 49.6 g (0.5 mole) of cyclohexylamine in 100 ml of methylenechloride. The temperature of the ensuing exothermal reaction rose from 24.5° to 42.5° C. thus keeping the solvent in reflux. After the reaction subsided, the reaction mixture, consisting of a slurry of white solids in a pale yellow solution, was heated to reflux with stirring. After standing overnight, the slurry was filtered, and the solution was stripped of the solvent and the oily residue distilled. The novel amidine (also called N'-cyclohexyl-N,N-dimethylbenzenecarboximidamide) was obtained as a colorless oil, boiling between 78° and 79° C. at 0.04 mm of mercury pressure and having a refractive index of nD 21.6, 1.5400, in 56.0 g corresponding to a 49% yield. Proton nmr infrared and elemental analysis confirmed its proposed structure.

後処理

  1. additionwas added dropwise
  2. customThe temperature of the ensuing exothermal reaction
  3. customrose from 24.5° to 42.5° C.
  4. temperaturein reflux
  5. temperaturewas heated
  6. temperatureto reflux
  7. filtrationthe slurry was filtered
  8. distillationthe oily residue distilled

出典と根拠

ORDレコード
ord-71d6fecc53b142e4bf090a1a1c596bf6
出典データセット
uspto-grants-1982_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04353830

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート