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

HRID 984492ノート

反応式

HRID 984492 の反応式
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]

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-8262694632d1443c9d51f89e356560ea
出典データセット
uspto-grants-2005_03
特許番号
US06867203B2

反応ノート

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