تفاعل #991902

ord-3f927c0a3bf04fb4b4bde1265d5024d0

معادلة التفاعل

[Na]
sodium
CCOC(=O)C(C)(C)O
ethyl α-hydroxyisobutyrate
NC(N)=O
urea
CC1(C)NC(=O)NC1=O
5,5-dimethylhydantoin
المردود 52.7%

الكواشف

لا شيء

المذيبات

ظروف التفاعل

درجة الحرارة
100°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.DISTILLATIONIn a 5-liter three neck distillation flask
  2. 2
    درجة الحرارةThe mixture was heated
  3. 3
    workup.DISTILLATIONAfter ethanol and methanol were distilled off from the reaction mixture
  4. 4
    workup.ADDITION2 l of water was added
  5. 5
    استخلاصextracted twice with ethyl acetate
  6. 6
    تجفيفThe extract was dried with Glauber's salt
  7. 7
    ترشيحfiltered
  8. 8
    workup.DISTILLATIONThe solvent was distilled off from the
  9. 9
    استخلاصextract

الإجراء التجريبي

In a 5-liter three neck distillation flask were placed 1.5 l of ethanol, 92 g of metallic sodium, 472 g of ethyl α-hydroxyisobutyrate (4 mole), and 240 g of urea (4 mole). The mixture was heated and stirred on hot oil bath at 100° C. for 18 hours. After ethanol and methanol were distilled off from the reaction mixture and then 2 l of water was added therefor, the mixture was made acid with aqueous hydrochloric acid solution and then extracted twice with ethyl acetate. The extract was dried with Glauber's salt, and then filtered. The solvent was distilled off from the extract to obtain 270 g of 5,5-dimethylhydantoin having a melting point of 75° C.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04419443uspto-grants-1983_12