醋酸 → 2-Propenoic acid, 3-phenyl-, methyl ester

HRID 483266

反应方程式

HRID 483266 反应方程式
[Cl-].[Ba+2].[Cl-].[C:4]([OH:7])(=[O:6])[CH3:5].C=[CH:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1.N#N.O=O.[C]=O.[CH3:22]O>[Pd]>[C:4]([O:7][CH3:22])(=[O:6])[CH:5]=[CH:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1

参与物

7

反应物 5

HCID 176醋酸HCID 887(5BETA,17BETA)-17-羟基-17-(甲基-D3)-2'H-雄甾-2-烯并[3,2-C]吡唑-5'(1'H)-酮HCID 7501苯乙烯HCID 5360350氯化钡HCID 178514649HCID 178514649，化合物

产物 1

HCID 76442-Propenoic acid, 3-phenyl-, methyl ester

试剂、催化剂与溶剂 1

HCID 23938钯催化剂3 次

反应条件

温度
120 °C

实验过程

Into a Teflon inner-cylinder Hastelloy C autoclave of a capacity of 300 ml and equipped with a magnetic induction rotating stirrer, a reflux condenser, a gas inlet pipe and a liquid withdrawal pipe were charged 0.5% Pd/A.C. (0.5% by weight of palladium supported on active carbon) in an amount of 0.05 mmol as Pd, 20 mmol of cupric acetate, 20 mmol of barium chloride, 160 mmol of acetic acid, 70 ml of styrene and 30 ml of methanol, then, a mixed gas of nitrogen/oxygen/carbon monoxide (84.9/5.6/9.5 in volume ratio) was introduced to make the pressure inside the reaction system 20.0 kg/cm2G, and while maintaining this pressure and passing the mixed gas at a gas flow rate at the reactor outlet of 34.1 Nl/hr, the reaction temperature was gradually raised to 120° C. While passing the mixed gas under the same conditions, the reaction was effected for 3 hours. Very small amounts of the reaction mixture were withdrawn at 30 minutes' intervals and analyzed by gas chromatography, and also the gas composition was analyzed at the same intervals by subjecting a part of the gas phase coming out of the reflux condenser to gas chromatography. The amounts of methyl cinnamate formed at intervals are shown in FIG. 1.

后处理

  1. temperaturewhile maintaining this pressure
  2. customVery small amounts of the reaction mixture were withdrawn at 30 minutes' intervals

来源与证据

ORD记录
ord-e6693fca82cf4927aa81111f9d708209
来源数据集
uspto-grants-1986_03
专利号
US04578507

关联笔记

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