Potassium Iodide → HCID 178490256、化合物

HRID 1482629ノート

反応式

HRID 1482629 の反応式
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]

参加物

6

反応物 4

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

生成物 1

HCID 178490256HCID 178490256、化合物収率 68.1%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-4b8183a8bde34bdabc5321a33361e3ba
出典データセット
uspto-grants-2016_08
特許番号
US09415047B2

反応ノート

読み込み中…