Hydrochloric Acid → HCID 89781834, 화합물

HRID 1056081노트

반응식

HRID 1056081 반응식
F[C:2]1[C:3]([CH3:15])=[N:4][C:5]2[C:10]([N:11]=1)=[C:9]([C:12](=[O:14])[CH3:13])[CH:8]=[CH:7][CH:6]=2.[ClH:16]>>[Cl:16][C:2]1[C:3]([CH3:15])=[N:4][C:5]2[C:10]([N:11]=1)=[C:9]([C:12](=[O:14])[CH3:13])[CH:8]=[CH:7][CH:6]=2

참가 물질

3

반응물 2

HCID 313Hydrochloric AcidHCID 897818641-(3-Fluoro-2-methylquinoxalin-5-yl)ethanone

생성물 1

HCID 89781834HCID 89781834, 화합물수율 99%

실험 절차

1-(3-Fluoro-2-methylquinoxalin-5-yl)ethanone (126g, 2.00 g, 9.79 mmol) was treated with HCl (4.0 M solution in 1,4-dioxane; 24.49 ml, 98 mmol), and the homogeneous reaction was fitted with a drying tube. After 6 h the reaction was concentrated in vacuo, and the solid was taken up in DCM. Solid NaHCO3 was added cautiously with rapid stirring; and saturated aq. NaHCO3 was sequentially added cautiously with rapid stirring. The mixture was partitioned between saturated NaHCO3 and DCM. The aq. layer was extracted with DCM (2×), and the combined organics were dried over anhydrous Na2SO4, filtered, and concentrated in vacuo to give 1-(3-chloro-2-methylquinoxalin-5-yl)ethanone (254a, 99% yield) as an orange-brown solid. MS (ESI, pos. ion) m/z: 221.0 (M+1).

후처리

  1. customthe homogeneous reaction
  2. customwas fitted with a drying tube
  3. concentrationAfter 6 h the reaction was concentrated in vacuo
  4. additionSolid NaHCO3 was added cautiously with rapid stirring
  5. additionand saturated aq. NaHCO3 was sequentially added cautiously with rapid stirring
  6. customThe mixture was partitioned between saturated NaHCO3 and DCM
  7. extractionThe aq. layer was extracted with DCM (2×)
  8. dry with materialthe combined organics were dried over anhydrous Na2SO4
  9. filtrationfiltered
  10. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-f16ae66eed154580a2fca3f563947cb5
출처 데이터셋
uspto-grants-2016_07
특허 번호
US09394297B2

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