Ammonium Hydroxide → HCID 15053447、化合物

HRID 974613ノート

反応式

HRID 974613 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.[OH-].[NH4+:18]>O1CCCC1.O>[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]([NH2:18])=[O:11])[CH2:7]1

参加物

5

反応物 2

HCID 14923Ammonium HydroxideHCID 15042235HCID 15042235、化合物

生成物 1

HCID 15053447HCID 15053447、化合物収率 57.4%

試薬・触媒・溶媒 2

HCID 962Water溶媒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 treated while stirring with 3 ml (0.04 mole) of 57% ammonium hydroxide. After stirring for 18 hr, the reaction mixture was diluted with 200 ml of water and the solid which separated was collected by filtration, 6.6 g. Recrystallization from ethanol-water yielded 3.0 g of white granular crystals, m.p. 179°-184° C. A second recrystallization from isopropanol yielded 2.7 g (51.7%) of fine white crystals, m.p. 185°-187° C.

後処理

  1. customthe solid which separated
  2. filtrationwas collected by filtration, 6.6 g
  3. customRecrystallization from ethanol-water

出典と根拠

ORDレコード
ord-50b7716f384b409a80dc6cf6ad0406b6
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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