Sulfuric Acid → HCID 19001619, 화합물

HRID 486928

반응식

HRID 486928 반응식
[C:1](O)(=[S:3])[CH3:2].[O:5]1[C:16]2[C:8](=[CH:9][C:10](=[CH:14][CH:15]=2)[CH2:11]C=C)[O:7][CH2:6]1.[OH-].[Na+].S(=O)(=O)(O)O>C(O)C.O>[O:5]1[C:16]2[CH:15]=[CH:14][C:10]([CH2:11][CH2:2][CH2:1][SH:3])=[CH:9][C:8]=2[O:7][CH2:6]1

참가 물질

7

반응물 4

HCID 1118Sulfuric AcidHCID 5144SafroleHCID 14798Sodium HydroxideHCID 178418634HCID 178418634, 화합물

생성물 1

HCID 19001619HCID 19001619, 화합물수율 66.4%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

실험 절차

25 g of thioacetic acid was added to 53.5 g of safrole in portions, while stirring the mixture at a room temperature or under cooling with ice/water. The reaction was carried out for 30 minutes. A solution of 20 g of sodium hydroxide in a mixture comprising 100 ml of water and 200 ml of ethanol was added to the reaction mixture. The obtained mixture was heated under reflux for 20 minutes, cooled, neutralized with dilute sulfuric acid and extracted with 1 l of benzene. The extract was washed with water and the benzene layer was dried over anhydrous sodium sulfate and purified by silica gel column chromatography (hexane) to obtain 42.8 g of the title compound as a colorless oil.

후처리

  1. temperatureThe obtained mixture was heated
  2. temperatureunder reflux for 20 minutes
  3. temperaturecooled
  4. extractionextracted with 1 l of benzene
  5. washThe extract was washed with water
  6. dry with materialthe benzene layer was dried over anhydrous sodium sulfate
  7. custompurified by silica gel column chromatography (hexane)

출처 및 근거

ORD 기록
ord-bc49ae4e5efa440f81f3746c1ac1f30b
출처 데이터셋
uspto-grants-1994_03
특허 번호
US05292901

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