Potassium Iodide → HCID 178490256, 화합물

HRID 1482629노트

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HRID 1482629 반응식
ClCCC[N:5]1[C:9]2[CH:10]=[C:11]([O:14][CH3:15])[CH:12]=[CH:13][C:8]=2[N:7]=[N:6]1.[O:16]1[C:20]2[CH:21]=[CH:22][CH:23]=[CH:24][C:19]=2[C:18]([CH:25]2[CH2:30][CH2:29][NH:28][CH2:27][CH2:26]2)=[CH:17]1.[CH:31](N(C(C)C)CC)([CH3:33])[CH3:32].[I-].[K+]>C(#N)C>[O:14]([C:11]1[CH:12]=[C:13]([CH2:32][CH2:31][CH2:33][N:28]2[CH2:29][CH2:30][CH:25]([C:18]3[C:19]4[CH:24]=[CH:23][CH:22]=[CH:21][C:20]=4[O:16][CH:17]=3)[CH2:26][CH2:27]2)[C:8]2[N:7]=[N:6][NH:5][C:9]=2[CH:10]=1)[CH3:15]

참가 물질

6

반응물 4

HCID 4875Potassium IodideHCID 81531DiisopropylethylamineHCID 214720424-(Benzofuran-3-yl)-piperidineHCID 118386874N-(3-chloropropyl)-6-methoxyl benzotriazole

생성물 1

HCID 178490256HCID 178490256, 화합물수율 68.1%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

N-(3-chloropropyl)-6-methoxyl benzotriazole (0.06 mol) was dissolved into 150 ml of acetonitrile, 4-(3-benzofuranyl) piperidine (0.05 mol), diisopropylethylamine (0.2 mol) and potassium iodide (0.05 mol) were respectively added. The mixture was stirred for 10 min at ambient temperature, and then heated and refluxed to react for 15 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, purified, eluted with dichloromethane/methanol mixture to produce 12.40 g N-(3-(6-methoxyl benzotriazolyl)propyl)-4-(3-benzofuranyl)piperidine (I-102) with a yield of 68.1%. ESI-MS [M+H]+: m/z 409.2.

후처리

  1. additionwere respectively added
  2. temperatureheated
  3. temperaturerefluxed
  4. customto react for 15 hours
  5. temperatureThe mixture was cooled down to ambient temperature
  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/methanol mixture

출처 및 근거

ORD 기록
ord-4b8183a8bde34bdabc5321a33361e3ba
출처 데이터셋
uspto-grants-2016_08
특허 번호
US09415047B2

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