Dimethyl Sulfate → Methyl 6-methoxy-1-naphthoate

HRID 280484

반응식

HRID 280484 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][CH:12]=1)[C:9]([C:13]([OH:15])=[O:14])=[CH:8][CH:7]=[CH:6]2.[C:16](=O)([O-])[O-].[K+].[K+].S(OC)(OC)(=O)=O>CC(C)=O>[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][CH:12]=1)[C:9]([C:13]([O:15][CH3:16])=[O:14])=[CH:8][CH:7]=[CH:6]2

참가 물질

5

반응물 3

HCID 6497Dimethyl SulfateHCID 11430Potassium CarbonateHCID 44137086-Methoxy-1-naphthoic acid

생성물 1

HCID 10921906Methyl 6-methoxy-1-naphthoate수율 90.9%

시약·촉매·용매 1

HCID 180Acetone용매2회

실험 절차

A mixture of 9.1 g of 6-methoxynaphthoic acid and 7.2 g of anhydrous potassium carbonate in 45 ml of acetone was heated to 50°-55° C. for 15 minutes, and 4.5 ml of dimethyl sulfate were then slowly dripped in over a period of 15 minutes. The mixture was then heated at reflux for one hour and cooled to room temperature, after which all the acetone was stripped under vacuum. After workup, it was determined that the process resulted in the formation of 8.85 g of methyl 6-methoxynaphthoate having an HPLC purity of 83.3%.

후처리

  1. temperaturewas heated to 50°-55° C. for 15 minutes
  2. customwere then slowly dripped in over a period of 15 minutes
  3. temperatureThe mixture was then heated
  4. temperatureat reflux for one hour

출처 및 근거

ORD 기록
ord-cf08e29ea3514f6994e053f6eccc4c15
출처 데이터셋
uspto-grants-1986_05
특허 번호
US04590010

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