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Sodium Iodide → HCID 12899539、化合物

HRID 621561
ノート
印刷プレビュー

反応式

HRID 621561 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 84.2%

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 under stirring conditions. The reactions mixture is concentrated under a reduced pressure to obtain a viscous liquid, then 300 ml of 3% sodium hydrogencarbonate aqueous solution are added. The organic layer is extracted with chloroform and washed with water. After drying the chloroform layer, 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 reactions 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, chloroform
  7. customis 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-7c43a7bdc2c4467aab4cc9d06094cd98
出典データセット
uspto-grants-1989_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04824840

反応ノート

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