Methyl isothiocyanate → 1-Methyl-3-trifluoromethanesulphonylthiourea

HRID 34776

반응식

HRID 34776 반응식
[CH3:1][N:2]=[C:3]=[S:4].[F:5][C:6]([F:12])([F:11])[S:7]([NH2:10])(=[O:9])=[O:8].[OH-].[Na+]>CC(C)=O.O>[CH3:1][NH:2][C:3]([NH:10][S:7]([C:6]([F:12])([F:11])[F:5])(=[O:9])=[O:8])=[S:4]

참가 물질

6

반응물 3

HCID 11167Methyl isothiocyanateHCID 14798Sodium HydroxideHCID 79001Trifluoromethylsulfonamide

생성물 1

HCID 212988821-Methyl-3-trifluoromethanesulphonylthiourea수율 42.3%

시약·촉매·용매 2

HCID 180Acetone용매HCID 962Water용매

실험 절차

A solution of methylisothiocyanate (0.21 g.) in acetone (10 ml.) was added to a solution of trifluoromethanesulphonamide (0.45 g.) and sodium hydroxide (0.12 g.) in water (5 ml.), the mixture stirred at 60° for 18 hours and then evaporated to dryness. The residue was dissolved in water and the solution washed with ethyl acetate and then adjusted to pH 1 with concentrated hydrochloric acid. The mixture was treated with charcoal and filtered and the filtrate extracted with ethyl acetate. The combined ethyl acetate extracts were dried and evaporated to dryness and the residue recrystallized from petroleum ether (b.p. 60°-80°) to give 1-methyl-3-trifluoromethanesulphonylthiourea (0.27 g.), m.p. 88°-90°.

후처리

  1. customevaporated to dryness
  2. dissolutionThe residue was dissolved in water
  3. washthe solution washed with ethyl acetate
  4. additionThe mixture was treated with charcoal
  5. filtrationfiltered
  6. extractionthe filtrate extracted with ethyl acetate
  7. dry with materialThe combined ethyl acetate extracts were dried
  8. customevaporated to dryness
  9. customthe residue recrystallized from petroleum ether (b.p. 60°-80°)

출처 및 근거

ORD 기록
ord-fc4168b320ef4c72aa266708c2dd8f0a
출처 데이터셋
uspto-grants-1988_08
특허 번호
US04762932

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