Potassium Iodide → HCID 76283391, 화합물

HRID 1482596노트

반응식

HRID 1482596 반응식
Cl[CH2:2][CH2:3][CH2:4][N:5]1[C:9]2[CH:10]=[CH:11][CH:12]=[CH:13][C:8]=2[N:7]=[N:6]1.[F:14][C:15]1[CH:29]=[CH:28][C:18]2[C:19]([N:22]3[CH2:27][CH2:26][NH:25][CH2:24][CH2:23]3)=[N:20][O:21][C:17]=2[CH:16]=1.C(N(C(C)C)CC)(C)C.[I-].[K+]>C(#N)C>[F:14][C:15]1[CH:29]=[CH:28][C:18]2[C:19]([N:22]3[CH2:27][CH2:26][N:25]([CH2:2][CH2:3][CH2:4][N:5]4[C:9]5[CH:10]=[CH:11][CH:12]=[CH:13][C:8]=5[N:7]=[N:6]4)[CH2:24][CH2:23]3)=[N:20][O:21][C:17]=2[CH:16]=1

참가 물질

6

반응물 4

HCID 4875Potassium IodideHCID 81531DiisopropylethylamineHCID 52439381-(3-chloropropyl)-1H-1,2,3-benzotriazoleHCID 19805377HCID 19805377, 화합물

생성물 1

HCID 76283391HCID 76283391, 화합물수율 69.3%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

1-(3-chloropropyl)-1H-benzotriazole (7.02 g, 0.036 mol) was dissolved into 100 ml of acetonitrile, 6-fluoro-3-(piperazine-1-yl)benzisoxazole (6.6 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 7.9 g compound (I-37) with a yield of 69.3%. ESI-MS [M+H]+: m/z 380.2.

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-e3eca9ec50df4b53865731af8135c6c2
출처 데이터셋
uspto-grants-2016_08
특허 번호
US09415047B2

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