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1-Chloro-2-fluorobenzene → 1-Chloro-2-fluoro-3-(methylsulfanyl)benzene

HRID 1738348
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HRID 1738348 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[F:8].C([Li])CCC.[CH3:14][S:15]SC>O1CCCC1.O>[Cl:1][C:2]1[C:3]([F:8])=[C:4]([S:15][CH3:14])[CH:5]=[CH:6][CH:7]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 95831-Chloro-2-fluorobenzeneHCID 12232Dimethyl DisulfideHCID 178418339Butyllithium

생성물 1

HCID 178598251-Chloro-2-fluoro-3-(methylsulfanyl)benzene

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매2회

실험 절차

A solution of 10 g (grams) (76 mmol (millimoles)) of 1-chloro-2-fluorobenzene in 75 mL (milliliters) of dry tetrahydrofuran (THF) was cooled with a dry ice/acetone bath and 34 mL (84 mmol) of 2.5M butyllithium was added dropwise under a nitrogen blanket over 45 min with stirring and cooling. The resulting solution was stirred for 2 hours at -78° C. A solution of 8.1 mL (91 mmol) of dimethyl disulfide in 10 mL of dry THF was added with stirring over a 30-min period keeping the temperature below -65° C. The mixture was allowed to warm to ambient temperature for 1 hour. It was then diluted with 75 mL of water. The resulting mixture was extracted with diethyl ether and the ether extract was dried over sodium sulfate and concentrated by evaporation under reduced pressure to obtain a yellow oil. This oil was purified by flash chromatography on 230-400 mesh silica gel eluting with a hexane/ethyl acetate mixture to obtain 9.0 g (69 percent of theory) of the title compound as a light yellow oil.

후처리

  1. temperaturecooling
  2. stirringThe resulting solution was stirred for 2 hours at -78° C
  3. stirringwith stirring over a 30-min period
  4. customthe temperature below -65° C
  5. extractionThe resulting mixture was extracted with diethyl ether
  6. extractionthe ether extract
  7. dry with materialwas dried over sodium sulfate
  8. concentrationconcentrated by evaporation under reduced pressure
  9. customto obtain a yellow oil
  10. customThis oil was purified by flash chromatography on 230-400 mesh silica gel eluting with a hexane/ethyl acetate mixture

출처 및 근거

ORD 기록
ord-358ca9b8c8ec460bb9311936168c109b
출처 데이터셋
uspto-grants-1999_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05962690

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