Ammonium Hydroxide → HCID 15053447, 화합물

HRID 1032143노트

반응식

HRID 1032143 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-6a3133123b5a40ce9935733801a13a5b
출처 데이터셋
uspto-grants-1990_09
특허 번호
US04956359

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