Dimethylamine → HCID 23459454、化合物

HRID 2287126ノート

反応式

HRID 2287126 の反応式
[CH3:1][NH:2][CH3:3].[CH3:4][CH:5](OS(C)(=O)=O)[CH2:6][C:7]1([C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)[CH:12]=[CH:11][CH2:10][CH:9]=[CH:8]1>C1(C)C=CC=CC=1>[CH3:4][CH:5]([N:2]([CH3:3])[CH3:1])[CH2:6][C:7]1([C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)[CH:12]=[CH:11][CH2:10][CH:9]=[CH:8]1

参加物

4

反応物 2

HCID 674DimethylamineHCID 53747931Methanesulfonic acid 1-methyl-2-(1-phenyl-2,5-cyclohexadien-1-yl)-ethyl ester

生成物 1

HCID 23459454HCID 23459454、化合物

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

1.1 ml. (about 3 equivalents) of condensed dimethylamine are added at -10° C. to 1.5 g. of methanesulfonic acid 1-methyl-2-(1-phenyl-2,5-cyclohexadien-1-yl)-ethyl ester in 5 ml. of toluene. The mixture is then held at 150° C. in a pressure vessel for 16 hours. Subsequently, the mixture is cooled down and worked-up as follows: The toluene phase is washed with water, concentrated, treated with ether and 3 N aqueous hydrochloric acid and shaken out. The aqueous extract is made basic with concentrated ammonia and extracted with ether. There is obtained an oily residue which is chromatographed on a thick-layer plate with methylene chloride/methanol (10:1). There is obtained α,N,N-trimethyl-1-phenyl-2,5-cyclohexadien-1-ethylamine which is converted in the usual manner into the hydrochloride.

後処理

  1. additionare added at -10° C. to 1.5 g
  2. temperatureSubsequently, the mixture is cooled down
  3. washThe toluene phase is washed with water
  4. concentrationconcentrated
  5. additiontreated with ether and 3 N aqueous hydrochloric acid
  6. extractionThe aqueous extract
  7. extractionextracted with ether
  8. customThere is obtained an oily residue which
  9. customis chromatographed on a thick-layer plate with methylene chloride/methanol (10:1)

出典と根拠

ORDレコード
ord-5181bfaa88094d46a2707f254effd662
出典データセット
uspto-grants-1981_05
特許番号
US04269788

反応ノート

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