2'-b-C-Methyl-2-aMino-N6,N6-diMethyladenosine synthesis

Yield:1336975-57-5 70%

Reaction Conditions:

in 1,4-dioxane; for 2 h;

Steps:

6.5 Step 5. Preparation of Compound 100.

To a solution containing 152 (0.3 g, 1.0 mmol) and 1,4-dioxane (2 mL) was added dimethylamine solution (1 mL). The reaction was stirred for 2 h and concentrated in vacuo. The residue was purified on silica gel using methanol/DCM (1:40) as the eluent. Fractions containing the product were pooled and concentrated in vacuo to afford 100 (0.200 g, 70%) as a colorless powder.1H NMR (400 MHz, Methanol-d4) δ 8.10 (s, 1H), 5.95 (s, 1H), 4.24 (d, J = 8.7 Hz, 1H), 4.08- 3.99 (m, 2H), 3.91- 3.82 (m, 1H), 3.42 (s, 6H), 3.37 (s, 2H), 0.95 (s, 3H).

References:

WO2018/48937,2018,A1 Location in patent:Page/Page column 229; 231