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Water → [2-(3,4-Dichloro-phenyl)-ethyl]-methyl-amine

HRID 1106860
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HRID 1106860 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([CH:8]=[CH:9][C:10]=1[Cl:11])[CH2:5][CH2:6]O.CS(Cl)(=O)=O.O.[N:18]1C=CC=C[CH:19]=1>>[Cl:1][C:2]1[CH:3]=[C:4]([CH:8]=[CH:9][C:10]=1[Cl:11])[CH2:5][CH2:6][NH:18][CH3:19]
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참가 물질

5

반응물 4

HCID 962WaterHCID 1049PyridineHCID 31297Methanesulfonyl chlorideHCID 2445582-(3,4-Dichlorophenyl)ethanol

생성물 1

HCID 15072478[2-(3,4-Dichloro-phenyl)-ethyl]-methyl-amine

실험 절차

A portion (1 g, 5.23 mmol) of the 3,4-dichlorophenethyl alcohol produced in (1) above was dissolved in pyridine (10 ml) and methanesulfonyl chloride (0.61 ml, 7.85 mmol) was slowly added dropwise, followed by stirring at room temperature for 1 h and pouring into water. The mixture was subjected to extraction with ethyl acetate and concentrated under vacuum; the residue was dissolved in 50 ml of a solution of 40% methylamine in methanol and the solution was stirred overnight at room temperature, followed by concentration under vacuum. The residue was subjected to column chromatography using a 9:1 solvent system of chloroform and methanol as an eluent to yield the end compound 3,4-dichlorophenethyl-N-methylamine (0.76 g).

후처리

  1. extractionThe mixture was subjected to extraction with ethyl acetate
  2. concentrationconcentrated under vacuum
  3. dissolutionthe residue was dissolved in 50 ml of a solution of 40% methylamine in methanol
  4. stirringthe solution was stirred overnight at room temperature
  5. concentrationfollowed by concentration under vacuum

출처 및 근거

ORD 기록
ord-4052a10bfa22447e92e90311b06f574e
출처 데이터셋
uspto-grants-2000_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06057358

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