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Dimethylformamide → 5-[[3,5-Bis(1,1-dimethylethyl)-4-hydroxyphenyl]methylene]-3-[2-(methylthio)ethyl]-4-thiazolidinone

HRID 2937
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HRID 2937 반응식
[CH3:1][C:2]([C:5]1[CH:6]=[C:7]([CH:16]=[C:17]2NC(=O)C[S:18]2)[CH:8]=[C:9]([C:12]([CH3:15])([CH3:14])[CH3:13])[C:10]=1[OH:11])([CH3:4])[CH3:3].[H-].[Na+].[CH3:25][S:26][CH2:27]CCl.[CH3:30][N:31]([CH:33]=[O:34])[CH3:32]>C(OCC)C.Cl>[CH3:3][C:2]([C:5]1[CH:6]=[C:7]([CH:16]=[C:17]2[S:18][CH2:30][N:31]([CH2:32][CH2:25][S:26][CH3:27])[C:33]2=[O:34])[CH:8]=[C:9]([C:12]([CH3:14])([CH3:13])[CH3:15])[C:10]=1[OH:11])([CH3:1])[CH3:4]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 6228DimethylformamideHCID 109652-Chloroethyl methyl sulfideHCID 24758Sodium hydrideHCID 86752333[3,5-Bis(1,1-dimethylethyl)-4-hydroxyphenyl]methylene-4-thiazolidinone

생성물 1

HCID 537084395-[[3,5-Bis(1,1-dimethylethyl)-4-hydroxyphenyl]methylene]-3-[2-(methylthio)ethyl]-4-thiazolidinone

시약·촉매·용매 2

HCID 313
Hydrochloric Acid
용매
2회
HCID 3283Diethyl Ether용매

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온도
100 °C

실험 절차

26.7 g of 5-[[3,5-Bis(1,1-dimethylethyl)-4-hydroxyphenyl]methylene-4-thiazolidinone (i.e., the compound of Example 2) was dissolved in 418 ml of DMF to which was added 3.34 g of a 60% sodium hydride dispersion. The resultant mixture was stirred at 100° C. under an argon atmosphere. To this was added 8.33 ml of methylthioethyl chloride and the resulting black solution was stirred at 100° C. for 6 days. The material was allowed to cool to 30° C. after which insoluble material was filtered off. The solid was washed with DMF until its color was gone leaving a white solid which was discarded. The pH of the filtrate and washings was adjusted to 1.5 by the addition of 1N hydrochloric acid with stirring. The mixture was then diluted with a mixture of 1000 ml of diethyl ether and 500 ml of 1N hydrochloric acid which was then shaken and separated. The organic layer was washed with two portions of water and one portion of brine and subsequently dried over sodium sulfate, filtered, evaporated and chased with chloroform to give a black foam/oil. This material was triturated with about 75 ml of chloroform and then filtered and the insoluble solid was washed with additional chloroform until its brown color was gone. The filtrate was then loaded onto a silica gel column which was eluted with 8000 ml of a gradient of 10-30% ethyl acetate in hexane. The various fractions containing the desired product were combined and again loaded onto a silica gel column and eluted with 8000 ml of a gradient of 10-35% acetone in hexane. The fractions containing the desired product were recrystalled with hexane/ethyl acetate to give 1.2 g of the title compound as a tan/orange solid, m.p. 165.5°-168° C.

후처리

  1. temperatureto cool to 30° C. after which insoluble material
  2. filtrationwas filtered off
  3. washThe solid was washed with DMF until its color
  4. customwas gone leaving a white solid which
  5. stirringwith stirring
  6. stirringwas then shaken
  7. customseparated
  8. washThe organic layer was washed with two portions of water and one portion of brine
  9. dry with materialsubsequently dried over sodium sulfate
  10. filtrationfiltered
  11. customevaporated
  12. customto give a black foam/oil
  13. customThis material was triturated with about 75 ml of chloroform
  14. filtrationfiltered
  15. washthe insoluble solid was washed with additional chloroform until its brown color
  16. washwas eluted with 8000 ml of a gradient of 10-30% ethyl acetate in hexane
  17. additionThe various fractions containing the desired product
  18. washeluted with 8000 ml of a gradient of 10-35% acetone in hexane
  19. additionThe fractions containing the desired product

출처 및 근거

ORD 기록
ord-72199bbc97064ed2941895c9e2129ccc
출처 데이터셋
uspto-grants-1998_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05731336

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