Ammonia → 4-(5,6-dihydro-11H-imidazo[2,1-b][3]benzazepin-11-ylidene)-1-(4-pyridinylcarbonyl)piperidine

HRID 275277

반응식

HRID 275277 반응식
P(Cl)(Cl)Cl.[N:5]1[CH:6]=[CH:7][N:8]2[CH2:14][CH2:13][C:12]3[CH:15]=[CH:16][CH:17]=[CH:18][C:11]=3[C:10](=[C:19]3[CH2:24][CH2:23][N+:22]([O-])([C:25]([C:27]4[CH:32]=[CH:31][N:30]=[CH:29][CH:28]=4)=[O:26])[CH2:21][CH2:20]3)[C:9]=12.O.N>ClCCl>[N:5]1[CH:6]=[CH:7][N:8]2[CH2:14][CH2:13][C:12]3[CH:15]=[CH:16][CH:17]=[CH:18][C:11]=3[C:10](=[C:19]3[CH2:24][CH2:23][N:22]([C:25]([C:27]4[CH:32]=[CH:31][N:30]=[CH:29][CH:28]=4)=[O:26])[CH2:21][CH2:20]3)[C:9]=12

참가 물질

6

반응물 4

HCID 222AmmoniaHCID 962WaterHCID 24387Phosphorus trichlorideHCID 867484844-(5,6-dihydro-11H-imidazo[2,1-b][3]benzazepin-11-ylidene)-1-(4-pyridinylcarbonyl)-piperidine N1-oxide

생성물 1

HCID 152322214-(5,6-dihydro-11H-imidazo[2,1-b][3]benzazepin-11-ylidene)-1-(4-pyridinylcarbonyl)piperidine

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

반응 조건

온도
25 °C

실험 절차

A solution of phosphorous trichloride (0.25 ml)in dichloromethane (3 ml) was added to a solution of 4-(5,6-dihydro-11H-imidazo[2,1-b][3]benzazepin-11-ylidene)-1-(4-pyridinylcarbonyl)-piperidine N1 -oxide (B, 0.4 g) and dichloromethane (5 ml). The reaction mixture was allowed to stir overnight at 25° C. in an atmosphere of nitrogen, and was then poured onto a mixture of ice and water. The resulting mixture was basified with concentrated aqueous ammonia, and the aqueous layer was extracted with dichloromethane. The dried (magnesium sulfate), filtered extracts were concentrated to give 4-(5,6-dihydro-11H-imidazo[2,1-b][3]benzazepin-11-ylidene )-1-(4-pyridinylcarbonyl)piperidine (A, 0.34 g), m.p. 207°-209° C. from carbon tetrachloride. ##STR25##

후처리

  1. extractionthe aqueous layer was extracted with dichloromethane
  2. dry with materialThe dried (magnesium sulfate)
  3. filtrationfiltered extracts
  4. concentrationwere concentrated

출처 및 근거

ORD 기록
ord-144e1a9cb859414384f4d4df3fd25ea8
출처 데이터셋
uspto-grants-1995_02
특허 번호
US05393753

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