1-Phenylpiperazine → HCID 19003519、化合物

HRID 2259406ノート

反応式

HRID 2259406 の反応式
[Cl:1][C:2]1[CH:15]=[CH:14][C:5]2[N:6]([CH2:10][CH2:11][CH2:12]Cl)[C:7](=[O:9])[S:8][C:4]=2[CH:3]=1.C([O-])([O-])=O.[K+].[K+].[CH:22]1[CH:23]=[CH:24][C:25]([N:28]2[CH2:33][CH2:32][NH:31][CH2:30][CH2:29]2)=[CH:26][CH:27]=1>CN(C=O)C>[Cl:1][C:2]1[CH:15]=[CH:14][C:5]2[N:6]([CH2:10][CH2:11][CH2:12][N:31]3[CH2:32][CH2:33][N:28]([C:25]4[CH:26]=[CH:27][CH:22]=[CH:23][CH:24]=4)[CH2:29][CH2:30]3)[C:7](=[O:9])[S:8][C:4]=2[CH:3]=1

参加物

5

反応物 3

HCID 70961-PhenylpiperazineHCID 11430Potassium CarbonateHCID 190035086-Chloro-3-(3-chloropropyl)-2(3H)-benzothiazolone

生成物 1

HCID 19003519HCID 19003519、化合物収率 61.9%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A solution of compound (X) (3.71 g, 20 mmol), K2CO3 (3.31 g, 24 tool), phenylpiperazine (XIb) (3.24 g, 20 mmol), and KI (3.98 g, 24 mmol) in DMF (20 ml) was stirred at 100° C. for 5 hours and concentrated in vacuo. The residue was extracted with dichloromethane, washed with a saturated saline solution and dried over MgSO4. The dichloromethane layer was subjected to column chromatography on silica gel. The eluate eluted with dichloromethane/ethyl acetate (4/1) was recrystallized from ethyl ether to obtain compound (XIIb) (4.8 g, yield=61.9%) as colorless prism-shaped crystals.

後処理

  1. concentrationconcentrated in vacuo
  2. extractionThe residue was extracted with dichloromethane
  3. washwashed with a saturated saline solution
  4. dry with materialdried over MgSO4
  5. washThe eluate eluted with dichloromethane/ethyl acetate (4/1)
  6. customwas recrystallized from ethyl ether
  7. customto obtain compound (XIIb) (4.8 g, yield=61.9%) as colorless prism-shaped crystals

出典と根拠

ORDレコード
ord-b17b4fc29a584e418816b2000e236a1d
出典データセット
uspto-grants-1995_12
特許番号
US05473066

反応ノート

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