Potassium Carbonate → HCID 19799596, 화합물

HRID 1886669노트

반응식

HRID 1886669 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.[CH3:17][N:18]1[CH2:23][CH2:22][NH:21][CH2:20][CH2:19]1.C(=O)([O-])[O-].[K+].[K+].[C:30]([OH:37])(=[O:36])/[CH:31]=[CH:32]/[C:33]([OH:35])=[O:34]>O1CCCC1.O.C(O)(C)C>[C:30]([OH:37])(=[O:36])/[CH:31]=[CH:32]/[C:33]([OH:35])=[O:34].[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]([N:21]2[CH2:22][CH2:23][N:18]([CH3:17])[CH2:19][CH2:20]2)=[O:11])[CH2:7]1

참가 물질

8

반응물 4

HCID 11430Potassium CarbonateHCID 531671-MethylpiperazineHCID 444972Fumaric AcidHCID 15042235HCID 15042235, 화합물

생성물 1

HCID 19799596HCID 19799596, 화합물수율 95.9%

시약·촉매·용매 3

HCID 962Water용매HCID 3776Isopropanol용매2회HCID 8028Tetrahydrofuran용매

실험 절차

A stirred solution of 2.8 g (0.01 mole) of crude 3-(3,4-dichlorophenoxy)-1-azetidinecarbonyl chloride in 25 ml of tetrahydrofuran was treated with 1 g (0.01 mole) of 1-methylpiperazine then with 1.42 g (0.01 mole) of potassium carbonate. After stirring for 30 min, approximately 2 g of ice was added and stirring continued for 18 hr. The reaction mixture was diluted with 200 ml of water and an oil separated. Upon standing, this oil solidified and was collected by filtration, yielding 3.3 g of crude product. The solid was dissolved in 20 ml of isopropanol and treated with 1.16 g of fumaric acid dissolved in 25 ml of boiling isopropanol. The volume was reduced to 30 ml by heating under a stream of nitrogen and upon cooling, the precipitated salt was collected by filtration, yielding 1.35 g (95.9%) of white crystals, m.p. 187°-188° C.

후처리

  1. stirringstirring
  2. waitcontinued for 18 hr
  3. customan oil separated
  4. filtrationwas collected by filtration
  5. customyielding 3.3 g of crude product
  6. temperatureby heating under a stream of nitrogen
  7. temperatureupon cooling
  8. filtrationthe precipitated salt was collected by filtration

출처 및 근거

ORD 기록
ord-5ef637bec92f47398d2ae8f1be870f25
출처 데이터셋
uspto-grants-1992_09
특허 번호
US05151418

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