1-Phenylpiperazine → HCID 19003519, 화합물

HRID 2259406노트

반응식

HRID 2259406 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

HCID 19003519HCID 19003519, 화합물수율 61.9%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-b17b4fc29a584e418816b2000e236a1d
출처 데이터셋
uspto-grants-1995_12
특허 번호
US05473066

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