تفاعل #2021470

ord-3ea1b85939b2489daa9ce7360a239846

معادلة التفاعل

CC1(O)C2CC3CC(C2)CC1C3
2-methyl-2-adamantanol
CCN(CC)CC
triethylamine
C=C(C)C(=O)Cl
methacryloyl chloride
C=C(C)C(=O)OC1(C)C2CC3CC(C2)CC1C3
2-methyl-2-adamantyl methacrylate
المردود 75.0%

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.ADDITIONwas added
  2. 2
    أخرىto form a solution
  3. 3
    ترشيحAfter filtration
  4. 4
    غسيلthe organic layer was washed with 5% aqueous sodium hydrogen carbonate solution
  5. 5
    غسيلwashed twice with water
  6. 6
    تركيزThe organic layer was concentrated
  7. 7
    workup.DISTILLATIONdistilled under reduced pressure

الإجراء التجريبي

Into a reaction vessel were charged 83.1 parts of 2-methyl-2-adamantanol and 101 parts of triethylamine, and 200 parts of methyl isobutyl ketone was added thereto to form a solution. To this solution was added dropwise 78.4 parts of methacryloyl chloride (1.5 mole based on 2-methyl-2-adamantanol). The solution was stirred at room temperature for about 10 hours. After filtration, the organic layer was washed with 5% aqueous sodium hydrogen carbonate solution and then washed twice with water. The organic layer was concentrated and distilled under reduced pressure to give 2-methyl-2-adamantyl methacrylate represented by the following formula in 75% yield:

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US06383713B1uspto-grants-2002_05