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

HRID 2371747

反応式

HRID 2371747 の反応式
[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

参加物

5

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

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.

後処理

  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.

出典と根拠

ORDレコード
ord-b829f53ccb3b417f8b09860b96f2687d
出典データセット
uspto-grants-1992_03
特許番号
US05095014

関連ノート

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