Potassium Iodide → 1-(4-(4-(2-furyl)piperazine-1-yl)butyl)-1H-benzotriazole

HRID 1482601노트

반응식

HRID 1482601 반응식
Cl[CH2:2][CH2:3][CH2:4][CH2:5][N:6]1[C:10]2[CH:11]=[CH:12][CH:13]=[CH:14][C:9]=2[N:8]=[N:7]1.[O:15]1[CH:19]=[CH:18][CH:17]=[C:16]1[N:20]1[CH2:25][CH2:24][NH:23][CH2:22][CH2:21]1.C(N(C(C)C)CC)(C)C.[I-].[K+]>C(#N)C>[O:15]1[CH:19]=[CH:18][CH:17]=[C:16]1[N:20]1[CH2:21][CH2:22][N:23]([CH2:2][CH2:3][CH2:4][CH2:5][N:6]2[C:10]3[CH:11]=[CH:12][CH:13]=[CH:14][C:9]=3[N:8]=[N:7]2)[CH2:24][CH2:25]1

참가 물질

6

반응물 4

HCID 4875Potassium IodideHCID 81531DiisopropylethylamineHCID 34251071-(4-chlorobutyl)-1H-benzotriazoleHCID 197635771-(Furan-2-yl)piperazine

생성물 1

HCID 762836371-(4-(4-(2-furyl)piperazine-1-yl)butyl)-1H-benzotriazole수율 71.7%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

1-(4-chlorobutyl)-1H-benzotriazole (7.55 g, 0.036 mol) was dissolved into 100 ml of acetonitrile, 4-(2-furyl)piperazine (4.6 g, 0.03 mol), diisopropylethylamine (15.5 g, 0.12 mol) and potassium iodide (5.0 g, 0.03 mol) were respectively added. The mixture was stirred and mixed, then heated and refluxed to react for 20 hours. The mixture was cooled down to ambient temperature and filtered. The filtrate was concentrated to produce oily products, and treated by chromatography with neutral Al2O3 and purified, eluted with dichloromethane to produce 7.0 g compound (I-43) with a yield of 71.3%. ESI-MS [M+H]+: m/z 325.2.

후처리

  1. additionwere respectively added
  2. additionmixed
  3. temperatureheated
  4. temperaturerefluxed
  5. customto react for 20 hours
  6. filtrationfiltered
  7. concentrationThe filtrate was concentrated
  8. customto produce oily products
  9. additiontreated by chromatography with neutral Al2O3
  10. custompurified
  11. washeluted with dichloromethane

출처 및 근거

ORD 기록
ord-ee06ae36b71d41eeb2d7d6969e0f186d
출처 데이터셋
uspto-grants-2016_08
특허 번호
US09415047B2

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