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Sodium Iodide → HCID 18999734、化合物

HRID 2260136
ノート
印刷プレビュー

反応式

HRID 2260136 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

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

生成物 1

HCID 18999734HCID 18999734、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-32a30de06e4a44eb994681cbd10393e4
出典データセット
uspto-grants-1995_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05476848

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート