Methyl Chloride → UM-424

HRID 1733354노트

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HRID 1733354 반응식
[CH:1]([N:4]([CH2:6][CH:7]([OH:22])[CH2:8][O:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=1[C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1)[CH3:5])([CH3:3])[CH3:2].[CH3:23][Cl:24]>CC(C)=O>[Cl-:24].[C:16]1([C:11]2[CH:12]=[CH:13][CH:14]=[CH:15][C:10]=2[O:9][CH2:8][CH:7]([OH:22])[CH2:6][N+:4]([CH:1]([CH3:3])[CH3:2])([CH3:23])[CH3:5])[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1

참가 물질

4

반응물 2

HCID 6327Methyl ChlorideHCID 203012641-[([1,1'-Biphenyl]-2-yl)oxy]-3-[methyl(propan-2-yl)amino]propan-2-ol

생성물 1

HCID 194064UM-424

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

To a solution of 10.0 g (0.033 moles) of 1-(N-isopropyl-N-methylamino)-3-(2-phenylphenoxy)propan-2ol and 30 ml of acetone, placed in a pressure container cooled in a Dry Ice-acetone bath is added 30 ml of methyl chloride. The container is sealed and mixture stirred at room temperature for about 8 days, after which time the mixture is again cooled in a Dry Ice-acetone bath. The container is opened slowly to permit reduction of any excess pressure and the solvent and excess methyl chloride is removed by evaporation under reduced pressure. The material remaining is dissolved in 30 ml of absolute ethanol, which then is evaporated under reduced pressure. The latter procedure is repeated and the residue is crystallized from anhydrous acetone to afford [3-(2-phenylphenoxy)-2-hydroxypropyl]isopropyldimethylammonium chloride melting at about 124°-127° C. and represented structurally by the following formula ##STR7##

후처리

  1. temperaturecooled in a Dry Ice-acetone bath
  2. customThe container is sealed
  3. temperatureafter which time the mixture is again cooled in a Dry Ice-acetone bath
  4. customthe solvent and excess methyl chloride is removed by evaporation under reduced pressure
  5. dissolutionThe material remaining is dissolved in 30 ml of absolute ethanol
  6. customwhich then is evaporated under reduced pressure
  7. customthe residue is crystallized from anhydrous acetone

출처 및 근거

ORD 기록
ord-c9061d94b40741a3aff1e48c9f0ff787
출처 데이터셋
uspto-grants-1980_12
특허 번호
US04241088

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