Potassium Iodide → HCID 76283391、化合物

HRID 1482596ノート

反応式

HRID 1482596 の反応式
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

参加物

6

反応物 4

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

生成物 1

HCID 76283391HCID 76283391、化合物収率 69.3%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-e3eca9ec50df4b53865731af8135c6c2
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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