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

HRID 369576
ノート
印刷プレビュー

反応式

HRID 369576 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒2 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-b0ee5de67ce845d08ab6f2eb1edd7594
出典データセット
uspto-grants-2000_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06140271

反応ノート

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