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Sodium Hydroxide → HCID 23708595, 화합물

HRID 1379298
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HRID 1379298 반응식
[F:1][C:2]([F:18])([F:17])[C:3]1[CH:8]=[CH:7][CH:6]=[C:5]([CH3:9])[C:4]=1[S:10]([O:13]C(C)C)(=[O:12])=[O:11].[OH-].[Na+:20]>O1CCCC1.O>[F:18][C:2]([F:1])([F:17])[C:3]1[CH:8]=[CH:7][CH:6]=[C:5]([CH3:9])[C:4]=1[S:10]([O-:13])(=[O:11])=[O:12].[Na+:20]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 14798Sodium HydroxideHCID 11832867Isopropyl 2-trifluoromethyl-6-methylbenzenesulfonate2회

생성물 1

HCID 23708595HCID 23708595, 화합물수율 92.1%

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매

실험 절차

A solution of 83 g of the crude isopropyl 2-trifluoromethyl-6-methylbenzenesulfonate (which contained about 10% of isopropyl 2-trifluoromethylbenzenesulfonate) in 300 mL of tetrahydrofuran was treated with a solution of 24.8 g of 50% aqueous sodium hydroxide in 150 mL of water and heated to reflux for 4 hours, then stirred at room temperature overnight. The mixture was assayed by capillary GC (10 m DB-1, 100°-250° C. at 20° C./min) to ascertain that the isopropyl 2-trifluoromethyl-6-methylbenzenesulfonate was consumed. The tetrahydrofuran was removed in vacuo, then the remainder was poured into 100 mL of water and 200 mL of hexane. The aqueous phase was washed with hexane, then the water removed in vacuo to yield 71 g sodium 2-trifluoromethyl-6-methylbenzenesulfonate as a white solid.

후처리

  1. temperatureheated
  2. temperatureto reflux for 4 hours
  3. customwas assayed by capillary GC (10 m DB-1, 100°-250° C. at 20° C./min)
  4. customwas consumed
  5. customThe tetrahydrofuran was removed in vacuo
  6. additionthe remainder was poured into 100 mL of water and 200 mL of hexane
  7. washThe aqueous phase was washed with hexane
  8. customthe water removed in vacuo

출처 및 근거

ORD 기록
ord-962d6d7eb17c4ecdaae6666ad10fedf5
출처 데이터셋
uspto-grants-1997_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05670691

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