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Potassium Carbonate → HCID 20079712、化合物

HRID 1654159
ノート
印刷プレビュー

反応式

HRID 1654159 の反応式
[CH3:1][NH:2][CH2:3][CH2:4][C:5]1[CH:10]=[CH:9][C:8]([Cl:11])=[CH:7][CH:6]=1.C(=O)([O-])[O-].[K+].[K+].Br[CH2:19][CH:20]([CH3:23])[CH2:21][Cl:22]>CN(C)C=O>[Cl:11][C:8]1[CH:9]=[CH:10][C:5]([CH2:4][CH2:3][N:2]([CH2:19][CH:20]([CH3:23])[CH2:21][Cl:22])[CH3:1])=[CH:6][CH:7]=1
参加物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 11430Potassium CarbonateHCID 955661-Bromo-3-chloro-2-methylpropaneHCID 135897732-(4-Chlorophenyl)-N-methylethan-1-amine

生成物 1

HCID 20079712HCID 20079712、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

16.9 g (0.1 mol) of N-methyl-2-(4-chlorophenyl)ethylamine were dissolved in 30 ml of dimethylformamide and treated with 20.7 g (0.3 mol) of anhydrous potassium carbonate. The mixture was stirred at 5° and treated with 12.6 ml (0.11 mol) of 1-bromo-2-methyl-3-chloropropane, whereupon the mixture was stirred at 30° for a further 4 hours, the solvent was evaporated at 30° under reduced pressure and the residue was treated with water. The separated oil was extracted three times with ether. The organic extracts were dried over magnesium sulphate and evaporated under reduced pressure. The residual oil was distilled at 135°-140°/260 Pa, whereby there was obtained rac-4-chloro-N-(3-chloro-2-methylpropyl)-N-methylphenethylamine as a colourless oil which was used directly in the next step. MS: 260 (M)+.

後処理

  1. stirringwas stirred at 30° for a further 4 hours
  2. customthe solvent was evaporated at 30° under reduced pressure
  3. additionthe residue was treated with water
  4. extractionThe separated oil was extracted three times with ether
  5. dry with materialThe organic extracts were dried over magnesium sulphate
  6. customevaporated under reduced pressure
  7. distillationThe residual oil was distilled at 135°-140°/260 Pa

出典と根拠

ORDレコード
ord-3ccab5c8439e49d68700f4398631b8a7
出典データセット
uspto-grants-1995_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05405866

反応ノート

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