Dimethylamine → 2-Dimethylamino-1-isopropyl-1-pyrrolinium methyl sulfate

HRID 1278031ノート

反応式

HRID 1278031 の反応式
[CH:1]([N+:4]1[CH2:8][CH2:7][CH2:6][C:5]=1OC)([CH3:3])[CH3:2].[CH3:11][O:12][S:13]([O-:16])(=[O:15])=[O:14].[CH3:17][NH:18][CH3:19]>C1C=CC=CC=1>[CH:1]([N+:4]1[CH2:8][CH2:7][CH2:6][C:5]=1[N:18]([CH3:19])[CH3:17])([CH3:3])[CH3:2].[CH3:11][O:12][S:13]([O-:16])(=[O:15])=[O:14]

参加物

4

反応物 2

HCID 674DimethylamineHCID 867369371-Isopropyl-2-methoxy-1-pyrrolinium methyl sulfate

生成物 1

HCID 1784564382-Dimethylamino-1-isopropyl-1-pyrrolinium methyl sulfate

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

Add dropwise, with stirring, 161 g of 1-isopropyl-2-methoxy-1-pyrrolinium-methylsulfate to a solution of 43.8 g of dimethylamine in 283 ml of benzene. Subsequently, boil the resulting reaction mixture under reflux for 1.5 hours; separate off the heavy phase and wash it 4 times with, in each case, 50 ml of diethyl ether. Dry the washed product under a high vacuum to obtain 154 g (91% of theory) of the title compound as reddish oil.

後処理

  1. additionAdd dropwise
  2. customthe resulting reaction mixture
  3. temperatureunder reflux for 1.5 hours
  4. customseparate off the heavy phase
  5. washwash it 4 times with, in each case, 50 ml of diethyl ether
  6. customDry the washed product under a high vacuum

出典と根拠

ORDレコード
ord-5715bd107fcd4a7ea0beecccc82ae5df
出典データセット
uspto-grants-1981_07
特許番号
US04279918

反応ノート

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