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

HRID 566639
ノート
印刷プレビュー

反応式

HRID 566639 の反応式
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]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 61436Stannous chloride dihydrateHCID 98159152-Nitrophenyl trifluoromethyl sulfide

生成物 1

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

試薬・触媒・溶媒 2

HCID 313Hydrochloric Acid溶媒HCID 702Ethanol溶媒

反応条件

温度
100 °C

実験手順

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.).

後処理

  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

出典と根拠

ORDレコード
ord-3bf0986a95094df794209f16e30c6c5a
出典データセット
uspto-grants-2001_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06175042B1

反応ノート

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