Potassium Iodide → 1-(4-(4-(3-cyanophenyl)piperazine-1-yl)butyl)-1H-benzotriazole

HRID 1482598노트

반응식

HRID 1482598 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.[C:15]([C:17]1[CH:18]=[C:19]([N:23]2[CH2:28][CH2:27][NH:26][CH2:25][CH2:24]2)[CH:20]=[CH:21][CH:22]=1)#[N:16].C(N(C(C)C)CC)(C)C.[I-].[K+]>C(#N)C>[C:15]([C:17]1[CH:18]=[C:19]([N:23]2[CH2:28][CH2:27][N:26]([CH2:2][CH2:3][CH2:4][CH2:5][N:6]3[C:10]4[CH:11]=[CH:12][CH:13]=[CH:14][C:9]=4[N:8]=[N:7]3)[CH2:25][CH2:24]2)[CH:20]=[CH:21][CH:22]=1)#[N:16]

참가 물질

6

반응물 4

HCID 4875Potassium IodideHCID 81531DiisopropylethylamineHCID 34251071-(4-chlorobutyl)-1H-benzotriazoleHCID 114809021-(3-Cyanophenyl)piperazine

생성물 1

HCID 762833941-(4-(4-(3-cyanophenyl)piperazine-1-yl)butyl)-1H-benzotriazole수율 70.5%

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, 3-cyano phenylpiperazine (5.6 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 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 and purified, eluted with dichloromethane to produce 7.6 g compound (I-41) with a yield of 70.5%. ESI-MS [M+H]+: m/z 360.2.

후처리

  1. additionwere respectively added
  2. additionmixed
  3. temperatureheated
  4. temperaturerefluxed
  5. customto react for 15 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-57d7bc0cd97047cbbbbae1c320fe17e6
출처 데이터셋
uspto-grants-2016_08
특허 번호
US09415047B2

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