Methylamine → 3-(2-Chloro-4-fluorophenoxy)-N-methyl-1-azetidinecarboxamide

HRID 2371747

반응식

HRID 2371747 반응식
[Cl:1][C:2]1[CH:15]=[C:14]([F:16])[CH:13]=[CH:12][C:3]=1[O:4][CH:5]1[CH2:8][N:7]([C:9](Cl)=[O:10])[CH2:6]1.[CH3:17][NH2:18]>O1CCCC1.O>[Cl:1][C:2]1[CH:15]=[C:14]([F:16])[CH:13]=[CH:12][C:3]=1[O:4][CH:5]1[CH2:8][N:7]([C:9]([NH:18][CH3:17])=[O:10])[CH2:6]1

참가 물질

5

반응물 2

HCID 6329MethylamineHCID 150422343-(2-Chloro-4-fluorophenoxy)-1-azetidinecarbonyl chloride

생성물 1

HCID 150422183-(2-Chloro-4-fluorophenoxy)-N-methyl-1-azetidinecarboxamide

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매

실험 절차

A stirred solution of 2.9 g (0.011 mole) of 3-(2-chloro-4-fluorophenoxy)-1-azetidinecarbonyl chloride in 20 mL of tetrahydrofuran was treated with 4 mL (0.05 mole) of 40% aqueous monomethylamine and stirred for 16 hr. The reaction mixture was diluted with 200 mL of water. The solid which precipitated was collected by filtration (2.7 g). The crude product was recrystallized from benzene/ligroin yielding 2.4 g (84.3%) of fine white crystals, mp 139°-141° C.

후처리

  1. customThe solid which precipitated
  2. filtrationwas collected by filtration (2.7 g)
  3. customThe crude product was recrystallized from benzene/ligroin yielding 2.4 g (84.3%) of fine white crystals, mp 139°-141° C.

출처 및 근거

ORD 기록
ord-b829f53ccb3b417f8b09860b96f2687d
출처 데이터셋
uspto-grants-1992_03
특허 번호
US05095014

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