m-Chloroperbenzoic acid → 4,4-Difluoro-3-methyl-3-butenyl 2-methanesulfonyl-4-methylpyrimidine-5-carboxylate

HRID 917377

반응식

HRID 917377 반응식
[CH3:1][C:2]1[C:7]([C:8]([O:10][CH2:11][CH2:12][C:13]([CH3:17])=[C:14]([F:16])[F:15])=[O:9])=[CH:6][N:5]=[C:4](SC)[N:3]=1.Cl[C:21]1C=CC=C(C(OO)=O)C=1.[S:31]([O-:34])(O)=[O:32].[Na+]>C(Cl)(Cl)Cl>[CH3:21][S:31]([C:4]1[N:3]=[C:2]([CH3:1])[C:7]([C:8]([O:10][CH2:11][CH2:12][C:13]([CH3:17])=[C:14]([F:16])[F:15])=[O:9])=[CH:6][N:5]=1)(=[O:34])=[O:32]

참가 물질

5

반응물 3

HCID 70297m-Chloroperbenzoic acidHCID 23665763Sodium BisulfiteHCID 69178886HCID 69178886, 화합물

생성물 1

HCID 691816824,4-Difluoro-3-methyl-3-butenyl 2-methanesulfonyl-4-methylpyrimidine-5-carboxylate수율 92%

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

To 20 ml of chloroform was dissolved 1.10 g (3.8 mmol) of 4,4-difluoro-3-methyl-3-butenyl 4-methyl-2-(methylthio)pyrimidine-5-carboxylate, followed by the addition, in three portions, of 2.00 g (8.1 mmol) of 70% m-chloroperbenzoic acid under ice-cooling and stirring for 1 hour after warming to room temperature. An aqueous solution of sodium hydrogensulfite was added under ice-cooling and the mixture was filtered to fractionate an organic layer. The organic layer was washed with a saturated sodium hydrogencarbonate solution and water in this order, followed by drying over anhydrous magnesium sulfate, the addition of “Florisil” and filtering. The solution was concentrated at 40° C. under reduced pressure to obtain 1.13 g (yield: 92%) of 4,4-difluoro-3-methyl-3-butenyl 2-methanesulfonyl-4-methylpyrimidine-5-carboxylate.

후처리

  1. temperaturecooling
  2. temperaturecooling
  3. filtrationthe mixture was filtered
  4. washThe organic layer was washed with a saturated sodium hydrogencarbonate solution and water in this order
  5. dry with materialby drying over anhydrous magnesium sulfate
  6. additionthe addition of “Florisil”
  7. filtrationfiltering
  8. concentrationThe solution was concentrated at 40° C. under reduced pressure

출처 및 근거

ORD 기록
ord-ffa3667fcdf5442a91df2ab16e44f8f3
출처 데이터셋
uspto-grants-2007_09
특허 번호
US07273878B2

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