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4-Toluenesulfonyl chloride → 8-{4-[2-(6-Chloro-1-benzofuran-3-yl)ethyl]-1-piperazinyl}-quinoline

HRID 1178795
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HRID 1178795 반응식
[Cl:1][C:2]1[CH:13]=[CH:12][C:5]2[C:6]([CH2:9][CH2:10]O)=[CH:7][O:8][C:4]=2[CH:3]=1.C1(C)C=CC(S(Cl)(=O)=O)=CC=1.S(C1C=CC(C)=CC=1)([O-])(=O)=O.[N:36]1([C:42]2[CH:43]=[CH:44][CH:45]=[C:46]3[C:51]=2[N:50]=[CH:49][CH:48]=[CH:47]3)[CH2:41][CH2:40][NH:39][CH2:38][CH2:37]1.C(N(CC)C(C)C)(C)C>N1C=CC=CC=1.CS(C)=O>[Cl:1][C:2]1[CH:13]=[CH:12][C:5]2[C:6]([CH2:9][CH2:10][N:39]3[CH2:40][CH2:41][N:36]([C:42]4[CH:43]=[CH:44][CH:45]=[C:46]5[C:51]=4[N:50]=[CH:49][CH:48]=[CH:47]5)[CH2:37][CH2:38]3)=[CH:7][O:8][C:4]=2[CH:3]=1
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참가 물질

8

반응물 5

HCID 73974-Toluenesulfonyl chlorideHCID 81531DiisopropylethylamineHCID 85570p-ToluenesulfonateHCID 118307868-(1-piperazinyl)QuinolineHCID 236144432-(6-Chloro-1-benzofuran-3-yl)ethanol

생성물 1

HCID 114521428-{4-[2-(6-Chloro-1-benzofuran-3-yl)ethyl]-1-piperazinyl}-quinoline

시약·촉매·용매 2

HCID 679Dimethyl Sulfoxide용매HCID 1049Pyridine용매

실험 절차

To a stirred solution of 2-(6-chloro-1-benzofuran-3-yl)ethanol (980 mg, 5 mmol) in anhydrous pyridine (20 ml), p-toluenesulfonyl chloride (1.14 g, 6.0 mmol) was added. The reaction mixture was kept at 0° C. for 48 hrs and quenched with ice cold water. The reaction mixture was extracted with chloroform, washed well with water and dried over anhydrous MgSO4. It was filtered and concentrated. The crude product obtained was taken to next step without any purification. A mixture of tosylate (350 mg. 1 mmol) (obtained by the above mentioned process) and 8-piperazino-quinoline (213 mg, 1 mmol) was heat at 120° C. in DMSO in the presence of N,N-diisopropylethylamine (5 ml, excess) for 24 hrs. At the end, reaction mixture was quenched with water and extracted with chloroform. The organic layer was washed with water and dried over anhydrous MgSO4 and concentrated to dryness. The dark colored solid was purified by silica-gel column chromatography by eluting it initially with 70% ethyl acetate:hexane and then with 5% methanol:ethyl acetate. 8-{4-[2-(6-chloro-1-benzofuran-3-yl)ethyl]-1-piperazinyl}-quinoline was isolated as a yellow oil. Yield: 120 mg (30%); (M+H): 392; 1HNMR (400 MHz, CDCl3):δ 8.82˜8.81 (dd, J1=1.7 Hz, J2=1.7 Hz, 1H); 8.40˜8.20 (dd, J1=1.8 Hz, J2=1.8 Hz, 1H); 7.46˜6.92 (m, 8H); 3.50˜2.70 (m, 12H).

후처리

  1. customquenched with ice cold water
  2. extractionThe reaction mixture was extracted with chloroform
  3. washwashed well with water
  4. dry with materialdried over anhydrous MgSO4
  5. filtrationIt was filtered
  6. concentrationconcentrated
  7. customThe crude product obtained
  8. customwas taken to next step without any purification
  9. customobtained by the
  10. customAt the end, reaction mixture
  11. customwas quenched with water
  12. extractionextracted with chloroform
  13. washThe organic layer was washed with water
  14. dry with materialdried over anhydrous MgSO4
  15. concentrationconcentrated to dryness
  16. customThe dark colored solid was purified by silica-gel column chromatography
  17. washby eluting it initially with 70% ethyl acetate

출처 및 근거

ORD 기록
ord-d6b5f130474946e7b36f94bc09a80ce8
출처 데이터셋
uspto-grants-2007_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07276603B2

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