Welcome to chemicalbook!
Chinese English Japanese Germany Korea
400-158-6606
Try our best to find the right business for you.
Do not miss inquiry messages Please log in to view all inquiry messages.

Welcome back!

5-CYANOGRAMINE synthesis

3synthesis methods
-

Yield:25514-67-4 94%

Reaction Conditions:

with glacial acetic acid in 1,4-dioxane at 20;

Steps:

25

Acetic acid (50 mL), formaldehyde (4.06 mL), and dimethylamine (9.01 mL) were added to a solution of 5-Cyanoindole (7. H g, 50.00 mmol) in 101.52 mL dioxane. The solution was stirred at room temperature overnight. The solution was evaporated in vacuo to give the crude active gramine. The crude active gramine was dissolved in water and adjusted pH to 11.0 with 5N NaOH. The product initially separated as oil but it solidified as a fine powder which was later collected by filtration, to give 9.67g (48.53 mmol, 94%) of product. TLC (silica Rf= 0.63, IPA/NH3/H20, 10:2:1 v/v/v). 1H NMR (DMSO) δ: 2.14 (s, 6H, 2CH3), 3.55 (s, 2H, CH2), 7.41 (m, 2H, Ar)5 7.53 (d, IH, Ar), 8.09 (s, IH, Ar), 11.50 (s, IH, NH).

References:

WO2007/75931,2007,A2 Location in patent:Page/Page column 41-42

5-CYANOGRAMINE Related Search: