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Sodium Iodide → HCID 12899539、化合物

HRID 569962
ノート
印刷プレビュー

反応式

HRID 569962 の反応式
Cl[CH2:2][CH2:3][CH2:4][O:5][C:6]1[CH:15]=[CH:14][CH:13]=[C:12]2[C:7]=1[CH2:8][CH2:9][C:10](=[O:16])[NH:11]2.[I-].[Na+].[CH2:19]([N:26]1[CH2:31][CH2:30][NH:29][CH2:28][CH2:27]1)[C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1.C(=O)([O-])O.[Na+]>C(N(CC)CC)C.CN(C)C=O.CC(C)=O>[CH2:19]([N:26]1[CH2:31][CH2:30][N:29]([CH2:2][CH2:3][CH2:4][O:5][C:6]2[CH:15]=[CH:14][CH:13]=[C:12]3[C:7]=2[CH2:8][CH2:9][C:10](=[O:16])[NH:11]3)[CH2:28][CH2:27]1)[C:20]1[CH:21]=[CH:22][CH:23]=[CH:24][CH:25]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 5238Sodium IodideHCID 759941-BenzylpiperazineHCID 516892Sodium BicarbonateHCID 12899139HCID 12899139、化合物

生成物 1

HCID 12899539HCID 12899539、化合物収率 84%

試薬・触媒・溶媒 3

HCID 180Acetone溶媒
HCID 6228
Dimethylformamide
溶媒
HCID 8471Triethylamine溶媒

実験手順

24 Grams of 5-(3-chloropropoxy)-3,4-dihydrocarbostyril and 17 g of sodium iodide are mixed with 300 ml of acetone and heated for 3 hours under refluxing conditions. Then, 300 ml of dimethylformamide, 12 g of triethylamine and 18 g of 4-benzylpiperazine are added thereto and the reaction is carried out at 60°-70° C. for 7 hours with stirring conditions. The reaction mixture is concentrated under a reduced pressure to obtain a viscous liquid, then 300 ml of 3% sodium hydrogencarbonate aqueous solution is added. The organic layer is extracted with chloroform and washed with water. After drying the chloroform layer, the chloroform is removed by distillation. The residue thus obtained is washed with ether and recrystallized from methanol to obtain 32 g (yield: 84%) of 5-[3-(4-benzylpiperazinyl)propoxy]-3,4-dihydrocarbostyril in the form of colorless needle-like crystals with a melting point of 157°-159° C.

後処理

  1. temperatureheated for 3 hours under refluxing conditions
  2. concentrationThe reaction mixture is concentrated under a reduced pressure
  3. customto obtain a viscous liquid
  4. extractionThe organic layer is extracted with chloroform
  5. washwashed with water
  6. dry with materialAfter drying the chloroform layer
  7. customthe chloroform is removed by distillation
  8. customThe residue thus obtained
  9. washis washed with ether
  10. customrecrystallized from methanol

出典と根拠

ORDレコード
ord-ab73fd6c939c48f7ac3652024bfcb2d5
出典データセット
uspto-grants-1988_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04734416

反応ノート

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