Methylamine → HCID 15042211, 화합물

HRID 2371740노트

반응식

HRID 2371740 반응식
[Cl:1][C:2]1[CH:15]=[CH:14][C:5]([O:6][CH:7]2[CH2:10][N:9]([C:11](Cl)=[O:12])[CH2:8]2)=[CH:4][CH:3]=1.[CH3:16][NH2:17]>O1CCCC1.O>[Cl:1][C:2]1[CH:15]=[CH:14][C:5]([O:6][CH:7]2[CH2:10][N:9]([C:11]([NH:17][CH3:16])=[O:12])[CH2:8]2)=[CH:4][CH:3]=1

참가 물질

5

반응물 2

HCID 6329MethylamineHCID 15042229HCID 15042229, 화합물

생성물 1

HCID 15042211HCID 15042211, 화합물수율 85.2%

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매

실험 절차

A stirred solution of 5 g (0.02 mole) of 3-(4-chlorophenoxy)-1-azetidinecarbonyl chloride in 20 ml of tetrahydrofuran was treated with 4.7 g (0.06 mole) of 40% aqueous monomethylamine. After stirring for 18 h, the reaction mixture was diluted with 200 ml of water and the solid which separated was collected by filtration, 5.7 g. Recrystallization from benzeneligroin was accomplished by adding magnesium sulfate to absorb the water which separated from the wet product. After filtering and cooling the hot filtrate, the precipitated solid was collected by filtration to yield 4.1 g (85%) of white crystals, mp 144°-145° C.

후처리

  1. customthe solid which separated
  2. filtrationwas collected by filtration, 5.7 g
  3. customRecrystallization from benzeneligroin
  4. additionby adding magnesium sulfate
  5. customto absorb the water which
  6. customseparated from the wet product
  7. filtrationAfter filtering
  8. temperaturecooling the hot filtrate
  9. filtrationthe precipitated solid was collected by filtration

출처 및 근거

ORD 기록
ord-b34e04bbbec64df8bb3acbc8a31dee58
출처 데이터셋
uspto-grants-1992_03
특허 번호
US05095014

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