3,4-Dimethoxytoluene → 3,4-Dimethoxy-6-(10-acetyloxydecanoyl)toluene

HRID 2254333노트

반응식

HRID 2254333 반응식
[C:1]([O:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][C:14]([OH:16])=O)(=[O:3])[CH3:2].ClC(Cl)C(OC(=O)C(Cl)Cl)=O.[CH3:28][O:29][C:30]1[CH:31]=[C:32]([CH3:38])[CH:33]=[CH:34][C:35]=1[O:36][CH3:37]>ClC(Cl)C>[CH3:28][O:29][C:30]1[CH:31]=[C:32]([CH3:38])[C:33]([C:14](=[O:16])[CH2:13][CH2:12][CH2:11][CH2:10][CH2:9][CH2:8][CH2:7][CH2:6][CH2:5][O:4][C:1](=[O:3])[CH3:2])=[CH:34][C:35]=1[O:36][CH3:37]

참가 물질

5

반응물 3

HCID 681263,4-DimethoxytolueneHCID 77772Acetic acid, 2,2-dichloro-, 1,1'-anhydrideHCID 1349720610-(Acetyloxy)decanoic acid

생성물 1

HCID 197452363,4-Dimethoxy-6-(10-acetyloxydecanoyl)toluene수율 84%

시약·촉매·용매 1

HCID 63651,1-Dichloroethane용매

반응 조건

온도
75 °C

실험 절차

In 50 ml of dichloroethane were dissolved 11.51 g (0.05 mole) of 10-acetyloxydecanoic acid and 14.39 g (0.06 mole) of dichloroacetic anhydride. To the resulting solution were added 9.89 g (0.065 mole) of 3,4-dimethoxytoluene and 0.71 g of boron trifluoridediethyl ether complex and the resulting mixture was then stirred at 75° C. for 5 hours. After completion of the reaction, the reaction solution was cooled and washed successively with water, 5% aqueous sodium carbonate solution and water. The organic layer was dried over anhydrous magnesium sulfate and then concentrated under reduced pressure to obtain 15.3 g of 3,4-dimethoxy-6-(10-acetyloxydecanoyl)toluene.

후처리

  1. customAfter completion of the reaction
  2. temperaturethe reaction solution was cooled
  3. washwashed successively with water, 5% aqueous sodium carbonate solution and water
  4. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  5. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-b18988843bc6437bb6721c7196e057be
출처 데이터셋
uspto-grants-1993_08
특허 번호
US05235068

반응 노트

불러오는 중…