تفاعل #1519079

ord-541908538fa04b72b2a190e0f6e9245b

معادلة التفاعل

CCCCC(CC)COC(=O)C(C#N)=C1C=C(C)OC(C)=C1
2-ethylhexyl (2,6-dimethyl-pyran-4-ylidene)cyanoacetate
CCCCC(CC)COC(=O)C(C#N)=C1C=C(C)N(CCCC)C(C)=C1
2-ethylhexyl (1-N-butyl-2,6-dimethyl-1H-pyridin-4-ylidene)cyanoacetate
المردود 128.3%

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىRemoval of the excess of butylamine at reduced pressure
  2. 2
    workup.WAITleft a orange oil which
  3. 3
    أخرىwas purified by FC (n-hexane/EtOAc 1:1)

الإجراء التجريبي

A solution of 0.30 g (1 mmol) of 2-ethylhexyl (2,6-dimethyl-pyran-4-ylidene)cyanoacetate (prepared as described in example 1) in 4 ml butylamine was refluxed at 80° C. for 1 h under nitrogen. Removal of the excess of butylamine at reduced pressure left a orange oil which was purified by FC (n-hexane/EtOAc 1:1) yielding 0.23 g (64%) of 2-ethylhexyl (1-N-butyl-2,6-dimethyl-1H-pyridin-4-ylidene)cyanoacetate as a slightly yellow solid.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07611696B2uspto-grants-2009_11