HRID892400

反应详情

EQUATION

反应方程式

HRID 892400 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2,2-Dimethoxypropane (418 parts), 3,3-bis(hydroxymethyl)-2-butanone (265 parts) and Amberlyst-15®, (40 parts) are combined in dichloromethane (1,320 parts) and the resultant suspension stirred vigorously at room temperature, ca. 1 hr. The spent resin is separated from the solution by filtration and the residual solvents removed in vacuo to yield a pale straw-colored liquid which can solidify upon standing. Yield is 87% of theory and analytical samples are recrystallized from ethyl ether, m.p. 48-50° C. Proton NMR and combustion analysis are consistent with those values predicted for the desired product. Combustion Analysis for C9H16O3 --Calculated: C, 62.8%; H, 9.4%. Found: C, 62.0%; H, 9.0%.

WORKUP

后处理

  1. customThe spent resin is separated from the solution by filtration
  2. customthe residual solvents removed in vacuo
  3. customto yield a pale straw-colored liquid which
  4. customYield is 87% of theory and analytical samples are recrystallized from ethyl ether, m.p. 48-50° C