Hydrochloric Acid → HCID 54283915, 화합물

HRID 1459447노트

반응식

HRID 1459447 반응식
[CH2:1]([O:5][C:6]1[CH:7]=[CH:8][C:9]([OH:15])=[C:10]([CH:14]=1)[C:11]([OH:13])=[O:12])[CH2:2][CH2:3][CH3:4].[CH2:16](Cl)[C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1.C(=O)([O-])[O-].[K+].[K+].[OH-].[Na+].Cl>C(O)C.O>[CH2:16]([O:15][C:9]1[CH:8]=[CH:7][C:6]([O:5][CH2:1][CH2:2][CH2:3][CH3:4])=[CH:14][C:10]=1[C:11]([OH:13])=[O:12])[C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1

참가 물질

8

반응물 5

HCID 313Hydrochloric AcidHCID 7503Benzyl ChlorideHCID 11430Potassium CarbonateHCID 14798Sodium HydroxideHCID 98157005-Butoxy-2-hydroxybenzoic acid

생성물 1

HCID 54283915HCID 54283915, 화합물

시약·촉매·용매 2

HCID 702Ethanol용매2회HCID 962Water용매3회

실험 절차

A suspension containing 1.9 g (9 mmol) of 5-butoxy-2-hydroxybenzoic acid, 3.85 g (30 mmol) of benzyl chloride and 5 g (36 mmol) of anhydrous potassium carbonate in 18 ml of anhydrous ethanol was boiled under reflux for 20 hours while stirring. The reaction mixture was cooled to room temperature and after adding 20 ml of water and thoroughly shaking, the three phases formed were separated. The medium phase was boiled under reflux with 1.1 g (27.5 mmol) of sodium hydroxide dissolved in 7 ml of ethanol and 5 ml of water for 2.5 hours under stirring. After cooling down the solution was mixed with 15 ml of water under cooling by ice, the pH value of the mixture was adjusted to 4 by adding 5M hydrochloric acid and stirred for 1 hour. After extracting the product with ethyl acetate and drying, the solution was evaporated to dryness under reduced pressure to give 1.5 g (55%) ot the aimed product, m.p.: 79°-82° C.

후처리

  1. temperatureunder reflux for 20 hours
  2. stirringthoroughly shaking
  3. customthe three phases formed
  4. customwere separated
  5. temperatureAfter cooling down the solution
  6. temperatureunder cooling by ice
  7. stirringstirred for 1 hour
  8. extractionAfter extracting the product with ethyl acetate
  9. customdrying
  10. customthe solution was evaporated to dryness under reduced pressure

출처 및 근거

ORD 기록
ord-38d975eab5a14de7a55907048ddf3577
출처 데이터셋
uspto-grants-1998_12
특허 번호
US05854250

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