Potassium Carbonate → HCID 13374747, 화합물

HRID 358222

반응식

HRID 358222 반응식
Cl.[Cl:2][C:3]1[CH:4]=[C:5]([N:9]2[CH2:14][CH2:13][NH:12][CH2:11][CH2:10]2)[CH:6]=[CH:7][CH:8]=1.Br[CH2:16][CH2:17][CH2:18][CH2:19]Cl.C(=O)([O-])[O-].[K+].[K+].[N:27]1[NH:28][C:29](=[O:36])[N:30]2[CH:35]=[CH:34][CH:33]=[CH:32][C:31]=12.[Na]>C(Cl)(Cl)Cl.C1(C)C(C)=CC=CC=1>[Cl:2][C:3]1[CH:4]=[C:5]([N:9]2[CH2:14][CH2:13][N:12]([CH2:16][CH2:17][CH2:18][CH2:19][N:28]3[C:29](=[O:36])[N:30]4[CH:35]=[CH:34][CH:33]=[CH:32][C:31]4=[N:27]3)[CH2:11][CH2:10]2)[CH:6]=[CH:7][CH:8]=1

참가 물질

7

반응물 4

HCID 11430Potassium CarbonateHCID 256811-(3-Chlorophenyl)piperazine monohydrochlorideHCID 813641-Bromo-4-chlorobutaneHCID 70507128Sodium 1,2,4-Triazolo[4,3-a]pyridin-3(2H)-one

생성물 1

HCID 13374747HCID 13374747, 화합물수율 43%

시약·촉매·용매 2

HCID 6212Chloroform용매HCID 7237O-Xylene용매

실험 절차

A mixture of 8.0 g. (0.0343 mole) of 1-(3-chlorophenyl)piperazine hydrocloride, 5.88 g. (0.0343 mole) of 1-bromo-4-chlorobutane, 9.48 g. (0.9686 mole) of finely powdered potassium carbonate, and 200 ml. of dry xylene was refluxed for 22 hr. To this mixture there was then added 5.39 g. (0.0343 mole) of sodium 1,2,4-triazolo[4,3-a]pyridin-3(2H)-one, and the resulting suspension was refluxed an additional 72 hr. The mixture was then cooled, diluted with 200 ml. of chloroform, stirred for 15 min. and filtered. The clear filtrate was concentrated to an oil (9.8 g.) under reduced pressure. The residue was recrystallized from ET2O--EtOH--CHCl3 to afford 2.31 g. (43%) of the desired product, m.p. 122°-123°.

후처리

  1. additionA mixture of 8.0 g
  2. additionTo this mixture there was then added 5.39 g
  3. temperatureThe mixture was then cooled
  4. additiondiluted with 200 ml
  5. filtrationfiltered
  6. concentrationThe clear filtrate was concentrated to an oil (9.8 g.) under reduced pressure
  7. customThe residue was recrystallized from ET2O
  8. customEtOH--CHCl3 to afford 2.31 g

출처 및 근거

ORD 기록
ord-9921cd8d05fa42deba4b5fc11d0e9396
출처 데이터셋
uspto-grants-1984_08
특허 번호
US04465683

연결된 노트

불러오는 중…