Ammonium Hydroxide → HCID 15053447, 화합물

HRID 1886650노트

반응식

HRID 1886650 반응식
[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

참가 물질

5

반응물 2

HCID 14923Ammonium HydroxideHCID 15042235HCID 15042235, 화합물

생성물 1

HCID 15053447HCID 15053447, 화합물수율 57.4%

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-0ae994d3bb5a4c3ba69c32038401fe89
출처 데이터셋
uspto-grants-1992_09
특허 번호
US05151418

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