Chlorotrimethylsilane → Methyl 5-chloro-2-(methylthio)pyrimidine-4-carboxylate

HRID 518780노트

반응식

HRID 518780 반응식
Cl[Si](C)(C)[CH3:3].[Cl:6][C:7]1[C:8]([C:15]([OH:17])=[O:16])=[N:9][C:10]([S:13][CH3:14])=[N:11][CH:12]=1>CO.ClCCl>[Cl:6][C:7]1[C:8]([C:15]([O:17][CH3:3])=[O:16])=[N:9][C:10]([S:13][CH3:14])=[N:11][CH:12]=1

참가 물질

5

반응물 2

HCID 6397ChlorotrimethylsilaneHCID 7257115-Chloro-2-(methylsulfanyl)pyrimidine-4-carboxylic acid

생성물 1

HCID 4736921Methyl 5-chloro-2-(methylthio)pyrimidine-4-carboxylate수율 95.1%

시약·촉매·용매 2

HCID 887Methanol용매HCID 6344Dichloromethane용매

실험 절차

16.0 g of chloro(trimethyl)silane are added dropwise to a solution of 6.2 g of 5-chloro-2-(methylsulfanyl)pyrimidine-4-carboxylic acid 1 in 100 ml of methanol and 100 ml of dichloromethane. The mixture is stirred at ambient temperature for 20 h, and then concentrated under vacuum. The residue is taken up with water and extracted with dichloromethane. The organic phase is dried over magnesium sulfate and concentrated under vacuum so as to obtain 6.3 g of methyl 5-chloro-2-(methylsulfanyl)pyrimidine-4-carboxylate 2 in the form of a brown oil.

후처리

  1. concentrationconcentrated under vacuum
  2. extractionextracted with dichloromethane
  3. dry with materialThe organic phase is dried over magnesium sulfate
  4. concentrationconcentrated under vacuum so as

출처 및 근거

ORD 기록
ord-a1bfda7f613a4a7d9be41445376a8292
출처 데이터셋
uspto-grants-2015_08
특허 번호
US09115140B2

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