Methylamine → 3-(3,4-Dichlorophenoxy)-N-methylazetidine-1-carboxamide

HRID 974607ノート

反応式

HRID 974607 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([CH:13]=[CH:14][C:15]=1[Cl:16])[O:5][CH:6]1[CH2:9][N:8]([C:10](Cl)=[O:11])[CH2:7]1.[CH3:17][NH2:18]>O1CCCC1>[Cl:1][C:2]1[CH:3]=[C:4]([CH:13]=[CH:14][C:15]=1[Cl:16])[O:5][CH:6]1[CH2:9][N:8]([C:10]([NH:18][CH3:17])=[O:11])[CH2:7]1

参加物

4

反応物 2

HCID 6329MethylamineHCID 15042235HCID 15042235、化合物

生成物 1

HCID 150422213-(3,4-Dichlorophenoxy)-N-methylazetidine-1-carboxamide

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

A solution of 5.6 g (0.02 mole) of 3-(3,4-dichlorophenoxy)-1-azetidinecarbonyl chloride in 20 ml of tetrahydrofuran was stirred while 5 ml (0.06 mole) of 40% aqueous methylamine was added slowly, stirring was continued for 18 hr. The reaction mixture was diluted with 200 ml of ice water, and the solid which formed was collected by filtration, 6.9 g. The crude wet solid was recrystallized from ethanol/water to yield 3.65 g (66.3%) of greenish-gray plate-like crystals, m.p. 158°-159° C.

後処理

  1. additionwas added slowly
  2. customthe solid which formed
  3. filtrationwas collected by filtration, 6.9 g
  4. customThe crude wet solid was recrystallized from ethanol/water
  5. customto yield 3.65 g (66.3%) of greenish-gray plate-like crystals, m.p. 158°-159° C.

出典と根拠

ORDレコード
ord-6f5707f449a545f9b0015457f8f61c6d
出典データセット
uspto-grants-1991_11
特許番号
US05068231

反応ノート

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