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Potassium Carbonate → HCID 20079712, 화합물

HRID 1464146
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HRID 1464146 반응식
[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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 955661-Bromo-3-chloro-2-methylpropaneHCID 135897732-(4-Chlorophenyl)-N-methylethan-1-amine

생성물 1

HCID 20079712HCID 20079712, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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)+.

후처리

  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

출처 및 근거

ORD 기록
ord-041b7352513d4d69a53b2e562b3419f3
출처 데이터셋
uspto-grants-1994_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05302727

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