Hydrochloric Acid → HCID 107657770, 화합물

HRID 629438노트

반응식

HRID 629438 반응식
F[C:2]1[C:10]([F:11])=[C:9]([CH3:12])[CH:8]=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].[OH-].[Na+].CS(C)=[O:17].Cl>O.C(OCC)(=O)C>[F:11][C:10]1[C:2]([OH:17])=[C:3]([CH:7]=[CH:8][C:9]=1[CH3:12])[C:4]([OH:6])=[O:5]

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 679Dimethyl SulfoxideHCID 14798Sodium HydroxideHCID 27741412,3-Difluoro-4-methylbenzoic acid

생성물 1

HCID 107657770HCID 107657770, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 8857Ethyl Acetate용매

반응 조건

온도
140 °C

실험 절차

A mixture of 2,3-difluoro-4-methylbenzoic acid (25.0 g), sodium hydroxide (23.2 g) and DMSO (250 mL) was stirred at 140° C. for 12 hr, and then overnight at room temperature, under argon atmosphere. To the reaction mixture was added 6M hydrochloric acid (100 mL) under ice-cooling. Ethyl acetate and water were added thereto at room temperature, the organic layer was separated, and the aqueous layer was extracted with ethyl acetate. The organic layers were combined, washed with water and saturated brine, and dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure to give the title compound (24.3 g). This compound was used in the next step without an additional purification.

후처리

  1. customovernight
  2. customat room temperature
  3. temperaturecooling
  4. customat room temperature, the organic layer was separated
  5. extractionthe aqueous layer was extracted with ethyl acetate
  6. washwashed with water and saturated brine
  7. dry with materialdried over anhydrous magnesium sulfate
  8. customthe solvent was evaporated under reduced pressure

출처 및 근거

ORD 기록
ord-6850f4b51435453d999b79af8b94edfb
출처 데이터셋
uspto-grants-2016_04
특허 번호
US09315458B2

반응 노트

불러오는 중…