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3-Chloro-2-methyl-1-propene → N-[1-methyl-1-(3-chlorophenyl)ethyl]-2-methyl-2-propenylamine

HRID 1707232
ノート
印刷プレビュー

反応式

HRID 1707232 の反応式
[CH3:1][C:2]([NH2:11])([C:4]1[CH:9]=[CH:8][CH:7]=[C:6]([Cl:10])[CH:5]=1)[CH3:3].C(=O)([O-])[O-].[K+].[K+].Cl[CH2:19][C:20]([CH3:22])=[CH2:21]>CN(C)C=O>[CH3:3][C:2]([NH:11][CH2:21][C:20]([CH3:22])=[CH2:19])([C:4]1[CH:9]=[CH:8][CH:7]=[C:6]([Cl:10])[CH:5]=1)[CH3:1]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 112413-Chloro-2-methyl-1-propeneHCID 11430Potassium CarbonateHCID 135695212-(3-Chlorophenyl)propan-2-amine

生成物 1

HCID 18962886N-[1-methyl-1-(3-chlorophenyl)ethyl]-2-methyl-2-propenylamine収率 75.8%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
85 °C

実験手順

To 15 ml of N,N-dimethylformamide were added 2.6 g of 1-methyl-1-(3-chlorophenyl)ethylamine, 2.0 g of potassium carbonate and 2.1 g of 3-chloro-2-methylpropene, and the solution was then stirred at 85° C. for 1 hour. After potassium carbonate was removed by filtration, 100 ml of water were added, followed by extraction with toluene. The resultant extract was dried over anhydrous sodium sulfate, and then concentrated by an evaporator. Afterward, silica gel column chromatography was done to obtain 2.6 g of the desired amine.

後処理

  1. customAfter potassium carbonate was removed by filtration, 100 ml of water
  2. additionwere added
  3. extractionfollowed by extraction with toluene
  4. extractionThe resultant extract
  5. dry with materialwas dried over anhydrous sodium sulfate
  6. concentrationconcentrated by an evaporator

出典と根拠

ORDレコード
ord-ab2f67676f654b0a8d6aeb85dda35479
出典データセット
uspto-grants-1994_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05352655

反応ノート

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