تفاعل #55856

ord-a490730804fa4e56a0d62e911c9482f5

ظروف التفاعل

درجة الحرارة
95°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةincrease in the temperature of the mixture to 100°-102° C.), the pH
  2. 2
    أخرىTotal consumption of 10% sodium hydroxide
  3. 3
    أخرىMost of the lead is precipitated with 10 g of sodium bicarbonate
  4. 4
    ترشيحhas been filtered off under suction

الإجراء التجريبي

1500 g of the 37% formalin solution of Example 1 (18.5 moles formaldehyde) and 491 g of cyclohexanone (5 moles) are heated with stirring to 95° C., followed by the addition of 56 g of a 50% aqueous solution of the formose used as co-catalyst in Example 1 of German Offenlegungsschrift No. 2,639,084 and 15 g of lead acetate trihydrate. The pH-value of the mixture is adjusted to 7.5 by the addition of 10% sodium hydroxide. After the reaction has started (increase in the temperature of the mixture to 100°-102° C.), the pH is kept between 6.5 and 7.0 by the addition of more sodium hydroxide. After about 20 minutes, the reaction is stopped at a residual formaldehyde content of 1.5% by cooling with ice water. Total consumption of 10% sodium hydroxide: 123 g. Most of the lead is precipitated with 10 g of sodium bicarbonate and the solution is fully desalted over ion exchangers after the deposit has been filtered off under suction. 800 g of a modified formose having a water content of 5.8% and a sugar content (expressed as glucose) of 37% are obtained.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04221876uspto-grants-1980_09