Hydrochloric Acid → 3-Chloro-4-hydroxy-2-(trifluoromethyl)benzaldehyde

HRID 984492노트

반응식

HRID 984492 반응식
C(Cl)(Cl)Cl.[C:5]([O-])([O-])=[O:6].[K+].[K+].[Cl:11][C:12]1[C:17]([C:18]([F:21])([F:20])[F:19])=[CH:16][CH:15]=[CH:14][C:13]=1[OH:22].Cl>O>[Cl:11][C:12]1[C:17]([C:18]([F:20])([F:21])[F:19])=[C:16]([CH:15]=[CH:14][C:13]=1[OH:22])[CH:5]=[O:6]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 6212ChloroformHCID 11430Potassium CarbonateHCID 27366012-Chloro-3-(trifluoromethyl)phenol

생성물 1

HCID 109331373-Chloro-4-hydroxy-2-(trifluoromethyl)benzaldehyde수율 11.7%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

Chloroform (6.7 g, 2.0 eq.) was added dropwise to a stirred mixture of Ca(OH)2 (8.95 g, 120 mmol.), K2CO3 (13.5 g, 98 mmol.), 2-chloro-3-(trifluoromethyl)phenol (5.0 g, 22 mmol.), and H2O (50 mL) at 60-70° C. over 2 h. The reaction mixture was cooled, and acidified with conc. HCl. The product was extracted into EtOAc and dried over Na2SO4. Solvent was evaporated, the crude product was separated and purified through a silica column, eluting with hexane and EtOAc (3:2) to give 580 mg (10%) of the title compound.

후처리

  1. temperatureThe reaction mixture was cooled
  2. extractionThe product was extracted into EtOAc
  3. dry with materialdried over Na2SO4
  4. customSolvent was evaporated
  5. customthe crude product was separated
  6. custompurified through a silica column
  7. washeluting with hexane and EtOAc (3:2)

출처 및 근거

ORD 기록
ord-8262694632d1443c9d51f89e356560ea
출처 데이터셋
uspto-grants-2005_03
특허 번호
US06867203B2

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