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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Hydrochloric Acid → 1'-[3-(3-chloro-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 1156771
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HRID 1156771 반응식
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[CH2:11][CH2:10][C:9]3[CH:12]=[CH:13][CH:14]=[CH:15][C:8]=3[N:7]([CH2:16][CH2:17][CH2:18][O:19]S(C)(=O)=O)[C:6]=2[CH:24]=1.[O:25]=[C:26]1[C:34]2([CH2:39][CH2:38][NH:37][CH2:36][CH2:35]2)[N:29]2[CH2:30][CH2:31][CH2:32][CH2:33][CH:28]2[NH:27]1.C(=O)([O-])[O-].[K+].[K+].[ClH:46]>C(O)C.CO.O>[OH2:19].[ClH:1].[ClH:46].[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[CH2:11][CH2:10][C:9]3[CH:12]=[CH:13][CH:14]=[CH:15][C:8]=3[N:7]([CH2:16][CH2:17][CH2:18][N:37]3[CH2:38][CH2:39][C:34]4([N:29]5[CH2:30][CH2:31][CH2:32][CH2:33][CH:28]5[NH:27][C:26]4=[O:25])[CH2:35][CH2:36]3)[C:6]=2[CH:24]=1
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참가 물질

8

반응물 4

HCID 313Hydrochloric AcidHCID 11430Potassium CarbonateHCID 130027121,2,3,5,6,7,8,8a-Octahydro-2-oxoimidazo[1,2-a]pyridine-3-spiro-4'-piperidineHCID 205339663-chloro-5-(3-methylsulfonyloxypropyl)-10,11-dihydro-5H-dibenz[b,f]azepine

생성물 1

HCID 704805021'-[3-(3-chloro-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

시약·촉매·용매 3

HCID 702Ethanol용매HCID 887Methanol용매HCID 962Water용매

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온도
60 °C

실험 절차

A mixture of 5 g of 3-chloro-5-(3-methylsulfonyloxypropyl)-10,11-dihydro-5H-dibenz[b,f]azepine, 4 g of 1,2,3,5,6,7,8,8a-octahydro-2-oxoimidazo[1,2-a]pyridine-3-spiro-4'-piperidine, 4 g of potassium carbonate and 4 g of water in 40 ml of ethanol is stirred at 60° C. for 4 hours. The upper layer is separated and concentrated, and the residue is dissolved in 100 ml of toluene. The toluene solution is washed with water, dried, concentrated to about 15 ml and allowed to stand. The precipitated crystals are collected by filtration and recrystallized from ethanol. The crystals thus obtained are dissolved in methanol, and methanolic hydrochloric acid is added to give 1'-[3-(3-chloro-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, m.p. 261° C. This product is dried at 120° C. under reduced pressure for 4 hours to give the anhydrous product as white crystals, m.p. 271° C., 4.3 g.

후처리

  1. customThe upper layer is separated
  2. concentrationconcentrated
  3. dissolutionthe residue is dissolved in 100 ml of toluene
  4. washThe toluene solution is washed with water
  5. customdried
  6. concentrationconcentrated to about 15 ml
  7. filtrationThe precipitated crystals are collected by filtration
  8. customrecrystallized from ethanol
  9. customThe crystals thus obtained

출처 및 근거

ORD 기록
ord-0957372320ad4ccf942f9fd35732ac7e
출처 데이터셋
uspto-grants-1982_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04337260

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