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Hydrochloric Acid → HCID 86760946, 화합물

HRID 730048
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HRID 730048 반응식
[Cl:1][C:2]1[CH:7]=[C:6]([C:8](=[N:18]O)[C:9]([C:11]2[CH:16]=[CH:15][C:14]([F:17])=[CH:13][CH:12]=2)=[O:10])[CH:5]=[CH:4][N:3]=1.Cl>CO.[Pd]>[ClH:1].[NH2:18][CH:8]([C:6]1[CH:5]=[CH:4][N:3]=[C:2]([Cl:1])[CH:7]=1)[C:9]([C:11]1[CH:12]=[CH:13][C:14]([F:17])=[CH:15][CH:16]=1)=[O:10]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 313Hydrochloric AcidHCID 1363357791-(2-Chloropyridin-4-yl)-2-(4-fluorophenyl)ethane-1,2-dione-1-oxime

생성물 1

HCID 86760946HCID 86760946, 화합물

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 887Methanol용매2회

실험 절차

With gentle heating, 22a (1.5 g; 5.4 mmol) was dissolved in methanol (15 ml). The solution was cooled to room temperature, HCl-containing methanol (20 ml) was added and the mixture was transferred into a two-necked flask. Pd—C 10% (150 mg) was introduced into the initial charge. The reaction vessel was evacuated using an oil pump, and H2 was then introduced via a gas inlet capillary (4×). At room temperature, the suspension was shaken in a closed three-necked flask under an atmosphere of H2 (240 strokes/min) until no more starting material could be detected by thin-layer chromatography (6 h). The suspension was filtered and the catalyst was washed with plenty of methanol. The combined filtrate was concentrated and the mustard-colored solid-amorphous residue was dried using an oil pump. The crude product was used without further purification for the next reaction step.

후처리

  1. additionwas added
  2. customthe mixture was transferred into a two-necked flask
  3. additioninitial charge
  4. customThe reaction vessel was evacuated
  5. additionwas then introduced via a gas inlet capillary (4×)
  6. customcould be detected by thin-layer chromatography (6 h)
  7. filtrationThe suspension was filtered
  8. washthe catalyst was washed with plenty of methanol
  9. concentrationThe combined filtrate was concentrated
  10. customthe mustard-colored solid-amorphous residue was dried
  11. customThe crude product was used without further purification for the next reaction step

출처 및 근거

ORD 기록
ord-03e67b17acf74eef872ca58154e409e3
출처 데이터셋
uspto-grants-2009_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07582660B2

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