Sodium Sulfite → 8-Cyclopentyl-2-methanesulfonyl-5-oxo-5,8-dihydro-pyrido[2,3-d]pyrimidine-6-carboxylic acid ethyl ester

HRID 1989025노트

반응식

HRID 1989025 반응식
[CH:1]1C=C(Cl)C=C(C(OO)=O)C=1.[CH2:12]([O:14][C:15]([C:17]1[C:18](=[O:34])[C:19]2[CH:24]=[N:23][C:22](SC)=[N:21][C:20]=2[N:27]([CH:29]2[CH2:33][CH2:32][CH2:31][CH2:30]2)[CH:28]=1)=[O:16])[CH3:13].[O-:35][S:36]([O-:38])=O.[Na+].[Na+]>C(Cl)Cl>[CH2:12]([O:14][C:15]([C:17]1[C:18](=[O:34])[C:19]2[CH:24]=[N:23][C:22]([S:36]([CH3:1])(=[O:38])=[O:35])=[N:21][C:20]=2[N:27]([CH:29]2[CH2:30][CH2:31][CH2:32][CH2:33]2)[CH:28]=1)=[O:16])[CH3:13]

참가 물질

5

반응물 3

HCID 24437Sodium SulfiteHCID 70297m-Chloroperbenzoic acidHCID 686785918-Cyclopentyl-2-methylsulfanyl-5-oxo-5,8-dihydro-pyrido[2,3-d]pyrimidine-6-carboxylic acid ethyl ester

생성물 1

HCID 686792108-Cyclopentyl-2-methanesulfonyl-5-oxo-5,8-dihydro-pyrido[2,3-d]pyrimidine-6-carboxylic acid ethyl ester

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

m-CPBA (0.45 g, 2.05 mmol of a 77% powder) was added to a solution of 8-cyclopentyl-2-methylsulfanyl-5-oxo-5,8-dihydro-pyrido[2,3-d]pyrimidine-6-carboxylic acid ethyl ester (0.27 g, 0.82 mmol) in DCM (5 mL). After 2 hours, a 10% solution of Na2SO3 (2 mL) was added and the mixture was partitioned between sat. NaHCO3 and DCM. The organic layer was dried (MgSO4) and concentrated to provide the title compound. Mass Spectrum (LCMS, ESI pos.) Calcd. For C16H19N3O5S: 365.10, found: (M+H) 366.1.

후처리

  1. customthe mixture was partitioned between sat. NaHCO3 and DCM
  2. dry with materialThe organic layer was dried (MgSO4)
  3. concentrationconcentrated

출처 및 근거

ORD 기록
ord-92099b7490ba46f5a1eacf62e929a6c9
출처 데이터셋
uspto-grants-2010_01
특허 번호
US07642270B2

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