4-Methylmorpholine → 6-[(8-chlorodibenz[b,f][1,4]oxazepin-10(11H)-yl)carbonyl]-N-(4-pyridinylmethyl)-2-pyridinecarboxamide, hydrochloride

HRID 37356

반응식

HRID 37356 반응식
[Cl:1][C:2]1[CH:16]=[CH:15][C:5]2[O:6][C:7]3[CH:14]=[CH:13][CH:12]=[CH:11][C:8]=3[CH:9]=[N:10][C:4]=2[CH:3]=1.[N:17]1[C:22]([C:23](Cl)=[O:24])=[CH:21][CH:20]=[CH:19][C:18]=1[C:26](Cl)=[O:27].CN1CCOCC1.[NH2:36][CH2:37][C:38]1[CH:43]=[CH:42][N:41]=[CH:40][CH:39]=1>C(Cl)(Cl)Cl>[ClH:1].[Cl:1][C:2]1[CH:16]=[CH:15][C:5]2[O:6][C:7]3[CH:14]=[CH:13][CH:12]=[CH:11][C:8]=3[CH2:9][N:10]([C:23]([C:22]3[N:17]=[C:18]([C:26]([NH:36][CH2:37][C:38]4[CH:43]=[CH:42][N:41]=[CH:40][CH:39]=4)=[O:27])[CH:19]=[CH:20][CH:21]=3)=[O:24])[C:4]=2[CH:3]=1

참가 물질

6

반응물 4

HCID 79724-MethylmorpholineHCID 773174-PyridinemethanamineHCID 773352,6-Pyridinedicarbonyl dichlorideHCID 8382678-Chloro-dibenz[b,f]-[1,4]oxazepine

생성물 1

HCID 1317190146-[(8-chlorodibenz[b,f][1,4]oxazepin-10(11H)-yl)carbonyl]-N-(4-pyridinylmethyl)-2-pyridinecarboxamide, hydrochloride

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

A solution of 8-chloro-dibenz[b,f][1,4]oxazepine (0.77 g), 2,6-pyridine-dicarbonyl chloride (0.68 g) and 4-methylmorpholine (0.367 mL) in CHCl3 (33 mL) was allowed to stand at ambient temperature for 16 hours. To this solution was added 4-(aminomethyl)pyridine (0.34 mL) and the mixture was allowed to stand at ambient temperature for 16 hours. The mixture was concentrated and the residue was extracted with ethyl acetate and saturated NaHCO3. The organic extract was concentrated and the residue chromatographed over silica gel using 50% ethyl acetate in hexane. Appropriate fractions were pooled and concentrated to give the free base of the title compound as a white solid. The HCl salt of the free base was made as described in Example 3.

후처리

  1. waitto stand at ambient temperature for 16 hours
  2. concentrationThe mixture was concentrated
  3. extractionthe residue was extracted with ethyl acetate and saturated NaHCO3
  4. extractionThe organic extract
  5. concentrationwas concentrated
  6. customthe residue chromatographed over silica gel using 50% ethyl acetate in hexane
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-f8ddeab8d46441a4b8fa8589c29649fd
출처 데이터셋
uspto-grants-1995_05
특허 번호
US05420270

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