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Pyridine → HCID 19856564, 화합물

HRID 2351037
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HRID 2351037 반응식
[F:1][C:2]([F:15])([F:14])[S:3]([O:6]S(C(F)(F)F)(=O)=O)(=[O:5])=[O:4].O[C:17]1[C:18](=[O:26])[N:19]([CH3:25])[CH:20]=[C:21]([O:23][CH3:24])[N:22]=1.N1C=CC=CC=1>C(Cl)Cl>[CH3:24][O:23][C:21]1[N:22]=[C:17]([O:6][S:3]([C:2]([F:15])([F:14])[F:1])(=[O:5])=[O:4])[C:18](=[O:26])[N:19]([CH3:25])[CH:20]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 1049PyridineHCID 67749Trifluoromethanesulfonic anhydrideHCID 178493752HCID 178493752, 화합물

생성물 1

HCID 19856564HCID 19856564, 화합물수율 68.6%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

62 g of trifluoromethanesulfonic acid anhydride are added dropwise to a suspension of 31.2 g of 3-hydroxy-5-methoxy-1-methylpyrazin-2-one, 15.8 g of pyridine and 500 ml of methylene chloride at 20°-25° C. The solution formed is stirred at 20°-25° C. for a further 2 hours, and 200 ml of ice-water are then added. The organic phase is separated off, washed with 10% sodium bicarbonate solution and water, dried over sodium sulfate and evaporated to give 39.5 g of 5-methoxy-1-methyl-3-trifluoromethylsulfonyloxy-pyrazin-2-one of melting point 107°-108° C.

후처리

  1. customThe solution formed
  2. customThe organic phase is separated off
  3. washwashed with 10% sodium bicarbonate solution and water
  4. dry with materialdried over sodium sulfate
  5. customevaporated

출처 및 근거

ORD 기록
ord-8a061ed533d5431ab514dfe584cc4e5c
출처 데이터셋
uspto-grants-1989_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04871853

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