Sodium hydride → 2-(2-Methylthioethoxy)nitrobenzene

HRID 4241

반응식

HRID 4241 반응식
[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]

참가 물질

5

반응물 3

HCID 24758Sodium hydrideHCID 738951-Fluoro-2-nitrobenzeneHCID 789252-(Methylthio)ethanol

생성물 1

HCID 539101632-(2-Methylthioethoxy)nitrobenzene

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

반응 조건

온도
40 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-4db7c84e1eb24c088f78a0ceb966e2c1
출처 데이터셋
uspto-grants-1988_02
특허 번호
US04725302

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