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

HRID 275277

反応式

HRID 275277 の反応式
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

参加物

6

反応物 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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

反応条件

温度
25 °C

実験手順

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##

後処理

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

出典と根拠

ORDレコード
ord-144e1a9cb859414384f4d4df3fd25ea8
出典データセット
uspto-grants-1995_02
特許番号
US05393753

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