Methanol → 3-Fluorosulfonyl-6-methoxypyridazine

HRID 1581493노트

반응식

HRID 1581493 반응식
CO[C:3]1[N:8]=[N:7][C:6]([SH:9])=[CH:5][CH:4]=1.[CH3:10][OH:11].[FH:12].[K].CC1CCC([OH:42])C/C/1=C/C=C1\CCCC2(C)C(C(/C=C/C(C(C)C)C)C)CCC\12.[OH2:43]>>[CH3:10][O:11][C:3]1[N:8]=[N:7][C:6]([S:9]([F:12])(=[O:42])=[O:43])=[CH:5][CH:4]=1

참가 물질

6

반응물 5

HCID 887MethanolHCID 962WaterHCID 5281010HCID 5281010, 화합물HCID 53443437Potassium fluoride, 99%, spray-driedHCID 178492798HCID 178492798, 화합물

생성물 1

HCID 110306363-Fluorosulfonyl-6-methoxypyridazine수율 74%

실험 절차

A mixture of 6-methoxy-pyridazine-3-thiol (7.1 g), methanol (100 mL), water (100 mL), and potassium hydrogen fluoride (39 g) was prepared and stirred at-10° C. for 30 minutes. Chlorine gas was bubbled into the mixture at a rate to ensure that the temperature did not exceed −10° C. The whitish-yellow reaction mixture was then poured into ice-cold water (50 mL) and the resulting white solid was filtered and air dried to afford the title compound (74%, 7.1 g); mp, 87-88° C.

후처리

  1. customwas prepared
  2. customChlorine gas was bubbled into the mixture at a rate
  3. customdid not exceed −10° C
  4. additionThe whitish-yellow reaction mixture was then poured into ice-cold water (50 mL)
  5. filtrationthe resulting white solid was filtered
  6. customair dried

출처 및 근거

ORD 기록
ord-9610e88b339c480b8105dd47a552b398
출처 데이터셋
uspto-grants-2004_05
특허 번호
US06730674B2

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