Potassium Carbonate → 1'-[3-(10,11-dihydro-5H-dibenz[b,f]azepin-5-yl)propyl]-1,2,3,5,6,7,8,8a-octahydro-2-oxo-imidazo[1,2-a]pyridine-3-spiro-4'-piperidine dihydrochloride monohydrate

HRID 1156770노트

반응식

HRID 1156770 반응식
[Cl:1][CH2:2][CH2:3][CH2:4][N:5]1[C:11]2[CH:12]=[CH:13][CH:14]=[CH:15][C:10]=2[CH2:9][CH2:8][C:7]2[CH:16]=[CH:17][CH:18]=[CH:19][C:6]1=2.[O:20]=[C:21]1[C:29]2([CH2:34][CH2:33][NH:32][CH2:31][CH2:30]2)[N:24]2[CH2:25][CH2:26][CH2:27][CH2:28][CH:23]2[NH:22]1.C(=O)([O-])[O-].[K+].[K+]>C(O)C>[OH2:20].[ClH:1].[ClH:1].[CH:16]1[C:7]2[CH2:8][CH2:9][C:10]3[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=3[N:5]([CH2:4][CH2:3][CH2:2][N:32]3[CH2:31][CH2:30][C:29]4([N:24]5[CH2:25][CH2:26][CH2:27][CH2:28][CH:23]5[NH:22][C:21]4=[O:20])[CH2:34][CH2:33]3)[C:6]=2[CH:19]=[CH:18][CH:17]=1

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 2867795-(3-Chloropropyl)-10,11-dihydro-5H-dibenz[b,f]azepineHCID 130027121,2,3,5,6,7,8,8a-Octahydro-2-oxoimidazo[1,2-a]pyridine-3-spiro-4'-piperidine

생성물 1

HCID 128312411'-[3-(10,11-dihydro-5H-dibenz[b,f]azepin-5-yl)propyl]-1,2,3,5,6,7,8,8a-octahydro-2-oxo-imidazo[1,2-a]pyridine-3-spiro-4'-piperidine dihydrochloride monohydrate수율 70%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A mixture of 23 g of 5-(3-chloropropyl)-10,11-dihydro-5H-dibenz[b,f]azepine, 15 g of 1,2,3,5,6,7,8,8a-octahydro-2-oxo-imidazo[1,2-a]pyridine-3-spiro-4'-piperidine and 10 g of anhydrous potassium carbonate in 100 ml of ethanol is boiled under reflux for 48 hours. The ethanol is then distilled off under reduced pressure. The residue is added to 80 ml of toluene, and the insoluble matter is filtered off. The filtrate is washed with two 50 ml portions of water, and alcoholic hydrochloric acid is added. The precipitated crystals are collected by filtration and recrystallized from methanol to give 1'-[3-(10,11-dihydro-5H-dibenz[b,f]azepin-5-yl)propyl]-1,2,3,5,6,7,8,8a-octahydro-2-oxo-imidazo[1,2-a]pyridine-3-spiro-4'-piperidine dihydrochloride monohydrate as white crystals, m.p. 258° C., 70% yield.

후처리

  1. temperatureunder reflux for 48 hours
  2. distillationThe ethanol is then distilled off under reduced pressure
  3. additionThe residue is added to 80 ml of toluene
  4. filtrationthe insoluble matter is filtered off
  5. washThe filtrate is washed with two 50 ml portions of water, and alcoholic hydrochloric acid
  6. additionis added
  7. filtrationThe precipitated crystals are collected by filtration
  8. customrecrystallized from methanol

출처 및 근거

ORD 기록
ord-0e82f1d9323948d2a4f1612cf807e026
출처 데이터셋
uspto-grants-1982_06
특허 번호
US04337260

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