Ammonia → 4-Methyl-sulfonylpyridine

HRID 18062

반응식

HRID 18062 반응식
CS([C:5]1[CH:10]=[CH:9][N:8]=[CH:7][CH:6]=1)(=O)=O.[CH3:11]SC1C=CN=CC=1.OO.N.[S:22]([O-:25])(O)=[O:23].[Na+]>[O-][W]([O-])(=O)=O.[Na+].[Na+].C(O)(=O)C.O>[CH3:11][C:5]1[CH:6]=[CH:7][NH:8][C:9](=[S:22](=[O:25])=[O:23])[CH:10]=1

참가 물질

9

반응물 5

HCID 222AmmoniaHCID 784Hydrogen PeroxideHCID 1409384-(Methylthio)pyridineHCID 2924874-MethanesulfonylpyridineHCID 23665763Sodium Bisulfite

생성물 1

HCID 865986304-Methyl-sulfonylpyridine

시약·촉매·용매 3

HCID 26052Sodium tungstate촉매HCID 176Acetic Acid용매HCID 962Water용매

실험 절차

4-Methylsulfonylpyridine may be prepared by carrying out the procedure as described in Example 20, starting with 14 g of sodium tungstate, 4 cm3 of water, 0.05 cm3 of 100% acetic acid, 3.3 g of 4-methylsulfanyl-pyridine, 6.5 cm3 of 30% hydrogen peroxide and then 0.25 cm3 of 32% aqueous ammonia and 1 cm3 of 37.5% aqueous solution of sodium hydrogen sulfite. The crude oil obtained is crystallized with 10 cm3 of diisopropyl ether, the crystals are filtered, drained and dried under reduced pressure (2.7 kPa). 2.6 g of 4-methyl-sulfonylpyridine are obtained in the form of white crystals.

후처리

  1. customThe crude oil obtained
  2. customis crystallized with 10 cm3 of diisopropyl ether
  3. filtrationthe crystals are filtered
  4. customdried under reduced pressure (2.7 kPa)

출처 및 근거

ORD 기록
ord-0849b5bd46324f2ca8a266329f580a42
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07741316B2

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