تفاعل #1585

ord-a7e627b3bd4d476c9aa919241c2544ff

معادلة التفاعل

O
water
Cn1c(=O)[nH]c(=O)n(-c2cc(N=c3sc(=O)n4n3CCCC4)c(F)cc2Cl)c1=O
1-{2-chloro-4-fluoro-5-[(tetrahydro-3-oxo-1H,3H-[1,3,4]thiadiazolo[3,4-a]pyridazin-1-ylidene)-amino]phenyl}-3-methyl-s-triazine-2,4,6(1H,3H,5H)-trione
O=C([O-])[O-].[K+].[K+]
potassium carbonate
C=CCBr
allyl bromide
C=CCn1c(=O)n(C)c(=O)n(-c2cc(N=c3sc(=O)n4n3CCCC4)c(F)cc2Cl)c1=O
title product
المردود 73.3%
C=CCn1c(=O)n(C)c(=O)n(-c2cc(N=c3sc(=O)n4n3CCCC4)c(F)cc2Cl)c1=O
1-Allyl-3-{2-chloro-4-fluoro-5-[(tetrahydro-3-oxo-1H,3H-[1,3,4]thiadiazolo[3,4-a]-pyridazine-1-ylidene)amino]phenyl}-5-methyl-s-triazine-2,4,6(1H,3H,5H)-trione
المردود 73.3%

المذيبات

ظروف التفاعل

درجة الحرارة
40°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    استخلاصThe aqueous mixture is extracted with ethyl acetate
  2. 2
    استخلاصThe organic extract
  3. 3
    غسيلis washed with water
  4. 4
    تجفيفdried over anhydrous magnesium sulfate
  5. 5
    تركيزconcentrated in vacuo

الإجراء التجريبي

A mixture of 1-{2-chloro-4-fluoro-5-[(tetrahydro-3-oxo-1H,3H-[1,3,4]thiadiazolo[3,4-a]pyridazin-1-ylidene)-amino]phenyl}-3-methyl-s-triazine-2,4,6(1H,3H,5H)-trione (1.00 g, 2.27 mmol), potassium carbonate (0.627 g, 4.54 mmol) and allyl bromide (0.329 g, 2.72 mmol) in acetone is stirred overnight at 40° C. and poured into water. The aqueous mixture is extracted with ethyl acetate. The organic extract is washed with water, dried over anhydrous magnesium sulfate, and concentrated in vacuo to give the title product as a white glass (0.8 g) which is identified by NMR spectral analyses.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05726126uspto-grants-1998_03