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Stannous chloride dihydrate → Benzenamine, 2-((trifluoromethyl)thio)-

HRID 566639
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HRID 566639 반응식
O.O.[Sn](Cl)Cl.[F:6][C:7]([S:10][C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=1[N+:17]([O-])=O)([F:9])[F:8]>Cl.C(O)C>[F:6][C:7]([S:10][C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=1[NH2:17])([F:9])[F:8]
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참가 물질

5

반응물 2

HCID 61436Stannous chloride dihydrateHCID 98159152-Nitrophenyl trifluoromethyl sulfide

생성물 1

HCID 67670Benzenamine, 2-((trifluoromethyl)thio)-수율 75.7%

시약·촉매·용매 2

HCID 313Hydrochloric Acid용매HCID 702Ethanol용매

반응 조건

온도
100 °C

실험 절차

A solution of 25.53 g of tin(II) chloride dihydrate in 40 ml of concentrated hydrochloric acid was added dropwise to a stirred solution of 5.05 g of 2-nitrophenyl trifluoromethyl sulfide, obtained according to Example 1, in 30 ml of ethanol. After the addition had ended, the mixture was heated to 100° C. and stirred at this temperature for 1.5 hours. The mixture was cooled, ethanol was evaporated off under reduced pressure, and the residue was poured into a mixture of 150 g of ice and 150 ml of 40% strength by weight aqueous sodium hydroxide solution. The product was extracted with ether. The combined ether extracts were dried over magnesium sulfate and concentrated under reduced pressure. Vacuum distillation of the residue gave 3.31 g (75.7% of theory) of 2-aminophenyl trifluoromethyl sulfide (boiling point 102-104° C. at 50 mbar, melting point: 30-31° C.).

후처리

  1. customobtained
  2. additionAfter the addition
  3. temperatureThe mixture was cooled
  4. customethanol was evaporated off under reduced pressure
  5. additionthe residue was poured into a mixture of 150 g of ice and 150 ml of 40% strength by weight aqueous sodium hydroxide solution
  6. extractionThe product was extracted with ether
  7. dry with materialThe combined ether extracts were dried over magnesium sulfate
  8. concentrationconcentrated under reduced pressure
  9. distillationVacuum distillation of the residue

출처 및 근거

ORD 기록
ord-3bf0986a95094df794209f16e30c6c5a
출처 데이터셋
uspto-grants-2001_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06175042B1

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