Hydrochloric Acid → HCID 178422611, 화합물

HRID 1956172노트

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HRID 1956172 반응식
C[S:2][C:3]1[C:8]([CH:9]2[C:17]3[C:12](=[CH:13][CH:14]=[CH:15][CH:16]=3)[CH2:11][C:10]2([CH3:19])[CH3:18])=[CH:7][N:6]=[CH:5][N:4]=1.C[S-].[Na+].Cl>CN(C)C=O>[SH:2][C:3]1[C:8]([CH:9]2[C:17]3[C:12](=[CH:13][CH:14]=[CH:15][CH:16]=3)[CH2:11][C:10]2([CH3:19])[CH3:18])=[CH:7][N:6]=[CH:5][N:4]=1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 4378561Sodium methanethiolateHCID 232269825-(2,2-Dimethyl-2,3-dihydro-1H-inden-1-yl)-4-(methylsulfanyl)pyrimidine

생성물 1

HCID 178422611HCID 178422611, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A mixture of 1.0 g (0.004 mol) of 4-methylthio-5-(2,2-dimethylindan-1-yl)pyrimidine and 1.4 g of sodium methanethiolate in 10 mL of N,N-dimethylformamide was prepared and heated to reflux with stirring for 1.5 hr. The mixture was cooled and was then added to 20 mL of 2N aqueous hydrochloric acid with stirring. The mixture obtained was extracted with 30 mL of ethyl acetate and the resulting organic solution was washed with water and then saturated aqueous sodium chloride. It was then dried over sodium sulfate and concentrated by evaporation under reduced pressure to obtain an oil. The oil was low pressure liquid chromatographed on silica gel eluting first with hexane to remove impurities and then with a 50:50 by volume mixture of ethyl acetate and hexane. The fractions containing the major component of the mixture were concentrated by evaporation under reduced pressure and the oil that was obtain solidified. The resulting 0.66 g (70 percent of theory) solids was the title compound melting at 184°-186° C.

후처리

  1. customwas prepared
  2. temperatureheated
  3. temperatureto reflux
  4. temperatureThe mixture was cooled
  5. stirringwith stirring
  6. customThe mixture obtained
  7. extractionwas extracted with 30 mL of ethyl acetate
  8. washthe resulting organic solution was washed with water
  9. dry with materialIt was then dried over sodium sulfate
  10. concentrationconcentrated by evaporation under reduced pressure
  11. customto obtain an oil
  12. customchromatographed on silica gel eluting first with hexane
  13. customto remove impurities
  14. additionwith a 50:50 by volume mixture of ethyl acetate and hexane
  15. additionThe fractions containing the major component of the mixture
  16. concentrationwere concentrated by evaporation under reduced pressure
  17. customthe oil that was obtain

출처 및 근거

ORD 기록
ord-0a6989c3c8c641c49c00bb1246f4bdd0
출처 데이터셋
uspto-grants-1998_07
특허 번호
US05780465

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