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Phosphorus oxychloride → Methyl (E)-3-(2,4,6-trimethoxyphenyl)acrylate

HRID 644101
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HRID 644101 반응식
[CH3:1][O:2][C:3]1[CH:8]=[C:7]([O:9][CH3:10])[CH:6]=[C:5]([O:11][CH3:12])[CH:4]=1.CO/[CH:15]=[CH:16]/[C:17]([O:19][CH3:20])=[O:18].P(Cl)(Cl)(Cl)=O>O.C(O)(=O)C>[CH3:12][O:11][C:5]1[CH:4]=[C:3]([O:2][CH3:1])[CH:8]=[C:7]([O:9][CH3:10])[C:6]=1/[CH:15]=[CH:16]/[C:17]([O:19][CH3:20])=[O:18]
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참가 물질

6

반응물 3

HCID 24813Phosphorus oxychlorideHCID 693011,3,5-TrimethoxybenzeneHCID 5323651Methyl 3-methoxyacrylate

생성물 1

HCID 23124870Methyl (E)-3-(2,4,6-trimethoxyphenyl)acrylate수율 91%

시약·촉매·용매 2

HCID 176Acetic Acid용매HCID 962Water용매2회

실험 절차

1.68 g of 1,3,5-trimethoxybenzene, 2.32 g of methyl trans-3-methoxyacrylate, 0.18 g of water and 6 mL of glacial acetic acid were mixed, 164 mg of phosphorus oxychloride was added into the mixture at an inner temperature of 25° C., the added mixture was stirred for 3 hours at the same temperature to cause a reaction. After completion of the reaction, 36 mL of water was added dropwise into the reaction liquid, and the precipitated crystals were filtrated. The crystals were washed with 20 vol % of aqueous methanol, then, dried to obtain 2.28 g of methyl trans-3-(2,4,6-trimethoxyphenyl)acrylate (white solid). Yield: 91%.

후처리

  1. customa reaction
  2. additionwas added dropwise into the reaction liquid
  3. filtrationthe precipitated crystals were filtrated
  4. washThe crystals were washed with 20 vol % of aqueous methanol
  5. customdried

출처 및 근거

ORD 기록
ord-52c7305466fd4b2294dea847e567c99c
출처 데이터셋
uspto-grants-2010_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07700642B2

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