Diethyl Ether → HCID 11159832、化合物

HRID 277564ノート

反応式

HRID 277564 の反応式
[CH:1]([O:6][CH3:7])([O:4][CH3:5])OC.C([CH2:10][C:11]([O-:13])=[O:12])=C.C1(=O)C=CC(=O)C=C1.B(F)(F)F.[O:26]([CH2:29]C)[CH2:27][CH3:28]>>[CH3:7][O:6][CH:1]([O:4][CH3:5])[CH2:28][CH:27]([O:26][CH3:29])[O:13][C:11](=[O:12])[CH3:10]

参加物

6

反応物 5

HCID 3283Diethyl EtherHCID 4650QuinoneHCID 6356Boron trifluorideHCID 9005Trimethyl orthoformateHCID 69710893-Butenoic acid, ion(1-)2 回

生成物 1

HCID 11159832HCID 11159832、化合物

反応条件

温度
30 °C

実験手順

A mixture of 56.00 g trimethyl ortho formate, 60.00 g vinylacetate, 0.75 g PdCl2(ACN)2, 0.60 g 1,4-benzoquinone, and 1.00 ml BF3*OEt2 was stirred at 30° C., and low boiling impurities were removed from the reaction mixture through the application of a slight vacuum. A fractionation column was installed to prevent losses of starting materials and/or products. After 2.3 hours, the ratio of 1,1,3,3-tetramethoxypropane to 1-acetoxy-1,3,3-trimethoxypropane, and the isomeric 1,3-diacetoxy-1,3-dimethoxy-propanes was determined by CG-analysis to be 1.0:2.4:1.3 on the basis of the FID-area-percentages. In a comparative experiment, without removal of low boiling impurities, the referring ratio was determined to be 1.0:1.48:0.50. Both reaction mixtures still contained an excess of vinylacetate.

後処理

  1. customlow boiling impurities were removed from the reaction mixture through the application of a slight vacuum
  2. customIn a comparative experiment, without removal of low boiling impurities
  3. customBoth reaction mixtures

出典と根拠

ORDレコード
ord-96361f58c4244f7cb626f288b6f32d34
出典データセット
uspto-grants-2002_03
特許番号
US06355844B1

反応ノート

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