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

HRID 1989025ノート

反応式

HRID 1989025 の反応式
[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]

参加物

5

反応物 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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-92099b7490ba46f5a1eacf62e929a6c9
出典データセット
uspto-grants-2010_01
特許番号
US07642270B2

反応ノート

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