Methacrylic Acid → 3,7-Dimethyloct-6-en-1-yl 2-methylprop-2-enoate

HRID 1107233노트

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HRID 1107233 반응식
[C:1]([OH:6])(=[O:5])[C:2]([CH3:4])=[CH2:3].[CH3:7][C:8](=[CH:10][CH2:11][CH2:12][CH:13]([CH2:15][CH2:16]O)[CH3:14])[CH3:9].C1(C)C=CC(S(O)(=O)=O)=CC=1>C1(C)C=CC=CC=1>[C:1]([O:6][CH2:16][CH2:15][CH:13]([CH2:12][CH2:11][CH:10]=[C:8]([CH3:9])[CH3:7])[CH3:14])(=[O:5])[C:2]([CH3:4])=[CH2:3]

참가 물질

5

반응물 3

HCID 4093Methacrylic AcidHCID 6101p-Toluenesulfonic acidHCID 8842Citronellol

생성물 1

HCID 162051083,7-Dimethyloct-6-en-1-yl 2-methylprop-2-enoate

시약·촉매·용매 1

HCID 1140Toluene용매

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온도
150 °C

실험 절차

24 g of methacrylic acid, 31 g of citronellol and 1.5 g of p-toluenesulfonic acid in 500 mL of toluene were heated to reflux at a oil temperature of 150° C. for 19 h. Subsequently, the reaction mixture was quenched by the addition of salt saturated sodium bicarbonate solution. The mixed solution was extracted with ether. The organic layers were combined and washed with salt saturated sodium bicarbonate solution, an aqueous solution of sodium hydride, and then salt saturated ammonium chloride solution, and then dried over salt saturated brine and sodium sulfate anhydrous. Finally, the resultant oily product was evaporated under reduced pressure to obtain citronellyl methacrylate.

후처리

  1. customSubsequently, the reaction mixture was quenched by the addition of salt saturated sodium bicarbonate solution
  2. extractionThe mixed solution was extracted with ether
  3. washwashed with salt saturated sodium bicarbonate solution
  4. dry with materialan aqueous solution of sodium hydride, and then salt saturated ammonium chloride solution, and then dried over salt saturated brine and sodium sulfate anhydrous
  5. customFinally, the resultant oily product was evaporated under reduced pressure

출처 및 근거

ORD 기록
ord-5a251c0ccdd143b1baf0e96d08592250
출처 데이터셋
uspto-grants-2000_05
특허 번호
US06060207

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