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Ethanol → HCID 23676786, 화합물

HRID 1492715
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HRID 1492715 반응식
Cl[C:2]1[CH:7]=[C:6]([C:8]([F:11])([F:10])[F:9])[CH:5]=[C:4]([C:12]([F:15])([F:14])[F:13])[N:3]=1.[S:16]([O-:19])([OH:18])=[O:17].[Na+:20].C(O)C>O>[F:9][C:8]([F:11])([F:10])[C:6]1[CH:5]=[C:4]([C:12]([F:15])([F:14])[F:13])[N:3]=[C:2]([S:16]([O-:19])(=[O:18])=[O:17])[CH:7]=1.[Na+:20]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 702EthanolHCID 147362352-Chloro-4,6-bis(trifluoromethyl)pyridineHCID 23665763Sodium Bisulfite

생성물 1

HCID 23676786HCID 23676786, 화합물수율 66.5%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A mixture of 2-chloro-4,6-bis(trifluoromethyl)pyridine (2.50 g, 10 mmol), sodium hydrogen sulfite (4.2 g, 40 mmol), ethanol (40 ml) and water (40 ml) was heated under reflux for 96.5 hours. The reaction mixture was evaporated to dryness under reduced pressure. To the residue, conc. hydrochloric acid was added and the mixture was again evaporated to dryness. The residued was extracted with methanol, and a methanol phase was filtered. The filtrate was evaporated to dryness under reduced pressure to obtain sodium 4,6-bis(trifluoromethyl)pyridine-2-sulfonate (2.11 g). Yield, 66%.

후처리

  1. temperaturewas heated
  2. temperatureunder reflux for 96.5 hours
  3. customThe reaction mixture was evaporated to dryness under reduced pressure
  4. additionTo the residue, conc. hydrochloric acid was added
  5. customthe mixture was again evaporated to dryness
  6. extractionThe residued was extracted with methanol
  7. filtrationa methanol phase was filtered
  8. customThe filtrate was evaporated to dryness under reduced pressure

출처 및 근거

ORD 기록
ord-cda1434a02ab404f8138736b285264a8
출처 데이터셋
uspto-grants-1994_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05374732

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