Sodium hydride → 2-(2-Methylthioethoxy)nitrobenzene

HRID 4241

Reaktionsgleichung

Reaktionsgleichung von HRID 4241
[OH:1][CH2:2][CH2:3][S:4][CH3:5].[H-].[Na+].F[C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=1[N+:15]([O-:17])=[O:16]>O1CCCC1>[CH3:5][S:4][CH2:3][CH2:2][O:1][C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=1[N+:15]([O-:17])=[O:16]

Komponenten

5

Reaktionsbedingungen

Temperatur
40 °C

Versuchsvorschrift

16.3 g of 2-hydroxyethylmethyl sulfide are added dropwise at 20°-25° C. to 8.5 g of a 55% NaH suspension in 150 ml of absolute tetrahydrofuran. The mixture is stirred for 1 hour at 20° C. and for 20 minutes at 40° C., and 25 g of 1-fluoro-2-nitrobenzene are subsequently added at 20° C. After the suspension has been stirred for 10 hours at 20° C., the tetrahydrofuran is distilled off in vacuo. Water is added to the residue, and extraction is repeatedly performed with ether. There is thus obtained an oil which can be used without further purification for the following hydrogenation stage.

Aufarbeitung

  1. stirringAfter the suspension has been stirred for 10 hours at 20° C.
  2. distillationthe tetrahydrofuran is distilled off in vacuo
  3. additionWater is added to the residue, and extraction
  4. customThere is thus obtained an oil which
  5. customcan be used without further purification for the following hydrogenation stage

Quellen und Nachweise

ORD-Eintrag
ord-4db7c84e1eb24c088f78a0ceb966e2c1
Quelldatensatz
uspto-grants-1988_02
Patentnummer
US04725302

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