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

HRID 854950

반응식

HRID 854950 반응식
[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

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 69339659ethyl 6-chloro-5,7-dimethyl-2-(trifluoromethyl)-2H-chromene-3-carboxylate

생성물 1

HCID 116092246-chloro-5,7-dimethyl-2-(trifluoromethyl)-2H-chromene-3-carboxylic Acid수율 95%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

실험 절차

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.

후처리

  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.

출처 및 근거

ORD 기록
ord-5a53b41b6b1e4752a26544cc668ef777
출처 데이터셋
uspto-grants-2007_08
특허 번호
US07259266B2

연결된 노트

불러오는 중…