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

HRID 1482601ノート

反応式

HRID 1482601 の反応式
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

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-ee06ae36b71d41eeb2d7d6969e0f186d
出典データセット
uspto-grants-2016_08
特許番号
US09415047B2

反応ノート

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