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Hydrazine → HCID 178478062, 화합물

HRID 341120
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HRID 341120 반응식
[Cl:1][C:2]1[N:7]=[C:6]([C:8]([C:10]2[C:15](F)=[N:14][CH:13]=[CH:12][N:11]=2)=O)[CH:5]=[CH:4][CH:3]=1.[NH2:17][NH2:18]>C1COCC1>[Cl:1][C:2]1[N:7]=[C:6]([C:8]2[C:10]3[C:15](=[N:14][CH:13]=[CH:12][N:11]=3)[NH:18][N:17]=2)[CH:5]=[CH:4][CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 9321HydrazineHCID 86677186(6-Chloropyridin-2-yl)(3-fluoropyrazin-2-yl)methanone

생성물 1

HCID 178478062HCID 178478062, 화합물수율 64%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of (6-chloro-2-pyridyl)-(3-fluoropyrazin-2-yl)methanone (1.12 g, 4.713 mmol) in THF (10 mL) was added hydrazine (1M in THF) (9.897 mL of 1 M, 9.897 mmol). Mixture turned orange and an exothermic reaction occurred, cream precipitate rapidly formed and mixture became difficult to stir. Stirred for 45 mins. Added sat. NaHCO3 solution and collected solid by filtration, washing solid with water then petrol. Solid then dried in vacuum oven overnight at 80° C. to leave title compound as an off-white solid (693 mg, 64%). 1H NMR (DMSO-d6) δ 7.58 (d, 1H), 8.07 (t, 1H), 8.52 (d, 1H), 8.70 (d, 1H), 8.80 (d, 1H), 14.55 (br s, 1H). ES+232.13.

후처리

  1. customan exothermic reaction
  2. customcream precipitate rapidly formed
  3. stirringStirred for 45 mins
  4. customAdded sat. NaHCO3 solution and collected solid
  5. filtrationby filtration
  6. washwashing solid with water
  7. customSolid then dried in vacuum oven overnight at 80° C.

출처 및 근거

ORD 기록
ord-e10b09116b264caea55e9360e5c88e69
출처 데이터셋
uspto-grants-2014_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08895740B2

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