Hydrochloric Acid → 6-chloro-5,7-dimethyl-2-(trifluoromethyl)-2H-chromene-3-carboxylic Acid

HRID 854950

反応式

HRID 854950 の反応式
[Cl:1][C:2]1[C:3]([CH3:22])=[C:4]2[C:9](=[CH:10][C:11]=1[CH3:12])[O:8][CH:7]([C:13]([F:16])([F:15])[F:14])[C:6]([C:17]([O:19]CC)=[O:18])=[CH:5]2.[OH-].[Na+].Cl>CCO.O>[Cl:1][C:2]1[C:3]([CH3:22])=[C:4]2[C:9](=[CH:10][C:11]=1[CH3:12])[O:8][CH:7]([C:13]([F:16])([F:14])[F:15])[C:6]([C:17]([OH:19])=[O:18])=[CH:5]2

参加物

6

実験手順

To a suspension of ethyl 6-chloro-5,7-dimethyl-2-(trifluoromethyl)-2H-chromene-3-carboxylate (4.00 g, 11.9 mmol) in 40 mL of EtOH was added a solution of NaOH (1.2 g, 30 mmol) in 18 mL of H2O. The reaction was heated at reflux for 1.5 h. Once cooled, the reaction was neutralized with 2 N HCl. The product that precipitated from solution was filtered and washed with H2O. After drying in the vacuum oven at 50° C., a pale yellow solid, 6-chloro-5,7-dimethyl-2-(trifluoromethyl)-2H-chromene-3-carboxylic acid, (3.46 g, 95%) was isolated.

後処理

  1. temperatureThe reaction was heated
  2. temperatureat reflux for 1.5 h
  3. temperatureOnce cooled
  4. customThe product that precipitated from solution
  5. filtrationwas filtered
  6. washwashed with H2O
  7. customAfter drying in the vacuum oven at 50° C.

出典と根拠

ORDレコード
ord-5a53b41b6b1e4752a26544cc668ef777
出典データセット
uspto-grants-2007_08
特許番号
US07259266B2

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