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Sodium Iodide → HCID 18999734, 화합물

HRID 2210813
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HRID 2210813 반응식
[CH2:1]1[CH:6]2[C:7]3[CH:19]=[CH:18][CH:17]=[CH:16][C:8]=3[CH2:9][C:10]3[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=3[N:5]2[CH2:4][CH2:3][NH:2]1.Cl[CH2:21][CH2:22][CH2:23][OH:24].C(=O)([O-])[O-].[K+].[K+].[I-].[Na+]>C(O)C>[CH2:1]1[CH:6]2[C:7]3[CH:19]=[CH:18][CH:17]=[CH:16][C:8]=3[CH2:9][C:10]3[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=3[N:5]2[CH2:4][CH2:3][N:2]1[CH2:21][CH2:22][CH2:23][OH:24]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 5238Sodium IodideHCID 11430Potassium CarbonateHCID 123133-Chloro-1-propanolHCID 115194Desmethylmianserin

생성물 1

HCID 18999734HCID 18999734, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

1.5 g of 1,2,3,4,10,14b-hexahydrodibenzo[c,f]pyrazino[1,2-a]azepine, 0.74 g of 3-chloropropanol, 2.32 g of potassium carbonate and 0.10 g of sodium iodide were added to 30 ml of ethanol, and the mixture was heated under reflux for 20 hours. At the end of this time, the reaction mixture was filtered, and then The solvent was removed from the filtrate by distillation under reduced pressure. The residue was then subjected to column chromatography through silica gel, and the desired compound was obtained as crystals from the fractions eluted with 5% by volume ethanol in chloroform; it was then recrystallized from ethyl acetate, to afford 1.28 g (69% yield) of the title compound, melting at 127°-128° C.

후처리

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 20 hours
  3. filtrationAt the end of this time, the reaction mixture was filtered
  4. customThe solvent was removed from the filtrate by distillation under reduced pressure

출처 및 근거

ORD 기록
ord-72765de7217c49f2b5dc0a4b5ac5123f
출처 데이터셋
uspto-grants-1995_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05461051

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