반응 #75003

반응 방정식

valeraldehyde

para-formaldehyde

sodium hydroxide

acetonitrile

valeraldehyde

→

2-propyl-2-hydroxymethyl-1,3-propanediol

반응 조건

후처리

1. 1
   온도To a heated
2. 2
   기타At this time, 8.4 grams of insoluble solid (sodium formate and excess para-formaldehyde) was removed by filtration
3. 3
   기타Removal of the actonitrile solvent
4. 4
   workup.WAITleft 13.3 grams (88%) of a viscous oil which
5. 5
   기타recrystallized from a chloroform-acetonitrile mixed solvent, m.p. 100°-101° C.

실험 절차

To a heated (ca. 60° C.), rapidly stirred mixture of 9.9 grams (0.33 mole) of para-formaldehyde, 4.8 grams (0.12 mole) of finely pulverized, anhydrous sodium hydroxide, and 100 mls. of acetonitrile, was added, drop-wise, 8.4 grams of valeraldehyde. After drop-wise addition of the valeraldehyde had been completed, the reaction mixture was maintained at 80° C. for a period of 1/2 hour. At this time, 8.4 grams of insoluble solid (sodium formate and excess para-formaldehyde) was removed by filtration and discarded. Removal of the actonitrile solvent left 13.3 grams (88%) of a viscous oil which was identified as the title compound, B.P. ca. 140° C.-155° C./0.4 mm Hg.; recrystallized from a chloroform-acetonitrile mixed solvent, m.p. 100°-101° C.

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