Sodium Sulfite → HCID 178474150, 화합물

HRID 1772910노트

반응식

HRID 1772910 반응식
C1C=C(Cl)C=C(C(OO)=[O:9])C=1.[CH3:12][C:13]1[CH:14]=[CH:15][C:16]([NH:19][C:20](=[O:22])[CH3:21])=[N:17][CH:18]=1.[O-]S([O-])=O.[Na+].[Na+]>C(Cl)Cl>[C:20]([NH:19][C:16]1[CH:15]=[CH:14][C:13]([CH3:12])=[CH:18][N+:17]=1[O-:9])(=[O:22])[CH3:21]

참가 물질

5

반응물 3

HCID 24437Sodium SulfiteHCID 70297m-Chloroperbenzoic acidHCID 818995N-(5-Methyl-2-pyridyl)acetamide

생성물 1

HCID 178474150HCID 178474150, 화합물수율 81%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

m-CPBA (75% in H2O, 89.6 g, 390 mmol) was added portion wise to a stirred solution of N-(5-methylpyridin-2-yl)acetamide (45.0 g, 300 mmol) in DCM (2.7 L) at rt, and the mixture stirred at rt for 4 h. 5% aqueous Na2SO3 (200 mL) was added slowly, the phases were separated and the organic layer washed with saturated NaHCO3, brine (100 mL), dried (MgSO4) and filtered. After concentration in vacuo purification by gradient column chromatography eluting with 2-5% MeOH in DCM yielded the title compound (37.5 g, 243 mmol) as a pale yellow solid.

후처리

  1. customthe phases were separated
  2. washthe organic layer washed with saturated NaHCO3, brine (100 mL)
  3. dry with materialdried (MgSO4)
  4. filtrationfiltered
  5. concentrationAfter concentration
  6. customin vacuo purification by gradient column chromatography
  7. washeluting with 2-5% MeOH in DCM

출처 및 근거

ORD 기록
ord-2582016e5df74018ba92924460f5d424
출처 데이터셋
uspto-grants-2016_02
특허 번호
US09249160B2

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