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Ethanol → Methacrolein diethylacetal

HRID 1769063
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HRID 1769063 반응식
O=[CH:2][C:3](=C)[CH3:4].C(O)C.C(O[CH:12]([O:16][CH2:17][CH3:18])[O:13][CH2:14][CH3:15])C>C1(C)C=CC(S(O)(=O)=O)=CC=1.C([O-])([O-])=O.[K+].[K+].C(Cl)Cl>[CH2:17]([O:16][CH:12]([O:13][CH2:14][CH3:15])[C:3](=[CH2:2])[CH3:4])[CH3:18]
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참가 물질

7

반응물 3

HCID 702EthanolHCID 6562MethacroleinHCID 31214Ethyl orthoformate

생성물 1

HCID 11194409Methacrolein diethylacetal수율 404.5%

시약·촉매·용매 3

HCID 6101p-Toluenesulfonic acid촉매HCID 11430Potassium Carbonate촉매HCID 6344Dichloromethane용매

실험 절차

p-Toluenesulfonic acid (1.14 g, 0.006 mol) was added to a mixture of methacrolein (42.35 g, 0.06 mol), ethanol (141.9 mL), CH2Cl2 (120 mL) and triethylorthoformate (130.6 mL, 0.785 mol). The mixture was stirred at room temperature for 3 days and then K2CO3 (2 g) was added. The mixture was stirred for 10 minutes, filtered, and then the filtrate was concentrated in vacuo. The residue was purified by distillation through a Vigreaux column at 130° C. to afford 35 g of methacrolein diethylacetal.

후처리

  1. stirringThe mixture was stirred for 10 minutes
  2. filtrationfiltered
  3. concentrationthe filtrate was concentrated in vacuo
  4. distillationThe residue was purified by distillation through a Vigreaux column at 130° C.

출처 및 근거

ORD 기록
ord-c242999875e24297bc3dcc641e9fa88f
출처 데이터셋
uspto-grants-1995_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05380729

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