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CAS No. : | 6622-92-0 | MDL No. : | MFCD00006105 |
Formula : | C6H8N2O | Boiling Point : | No data available |
Linear Structure Formula : | C4HN2(OH)(CH3)2 | InChI Key : | UQFHLJKWYIJISA-UHFFFAOYSA-N |
M.W : | 124.14 | Pubchem ID : | 135408640 |
Synonyms : |
|
Chemical Name : | 2,6-Dimethylpyrimidin-4-ol |
Signal Word: | Warning | Class: | |
Precautionary Statements: | P261-P305+P351+P338 | UN#: | |
Hazard Statements: | H315-H319-H335 | Packing Group: | |
GHS Pictogram: |
* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
65% | With iodine; sodium hydroxide; In water; at 80℃; for 2.0h; | Step A: 2,6-Dimethylpyrimidin-4-ol (5.0 g, 40 mmol) was dissolved in aqueous NaOH solution (50 mL, 1 M, 50 mmol). To the solution was added iodine (10.2 g, 40 mmol). The mixture was gradually heated to 80 C. and stirred for 2 h. After cooling the mixture to room temperature, acetic acid was added to adjust the pH ?6. A precipitate formed and was collected by filtration. The solid was washed with water and dried to give 5-iodo-2,6-dimethylpyrimidin-4-ol (6.51 g, 65%). MS m/z 251.2 [M+H]+. |
50.5 g (50%) | With sodium hydroxide; iodine; | Step 1 2,6-Dimethyl-5-iodo-4-hydroxypyrimidine A mechanically stirred mixture of 2,6-dimethyl-4-hydroxypyrimidine (50.0 g, 0.403 mol), iodine (102.2 g, 0.403 mol), and 1N NaOH (503 mL) was heated under reflux for 2 h. The mixture was extracted with CHCl3 (some product fell out of solution and was collected by filtration: 24.5 g). The extracts were dried MgSO4) and concentrated to give 40.9 g of an orange solid which contained starting material and product. Trituration with EtOAc gave 26.0 g of product. The total yield of product was 50.5 g (50%), mp 208-210 (dec). An analytical sample was recrystallized from EtOH, mp 216-218. 1 H NMR (DMSO-d6) delta2.21 (s, 3H), 2.39 (s, 3H), 12.58 (br s, 1H). Anal. calcd for C6 H7 IN2 O: C, 28.82; H, 2.82; N, 11.20; Found: C, 28.85; H, 2.76; N, 10.98. |
With iodine; sodium hydroxide; In water; at 120℃; for 2.0h; | (2) 5-iodo-2,6-dimethylpyrimidin-4-ol (326-2)The crude compound 326-1 (25.6 g) was dissolved in a 1.25 N sodium hydroxide aqueous solution (140 ml). Iodine (19.9 g) was added to the solution, and the obtained mixture was then stirred at 120 C. for 2 hours. The temperature of the reaction solution was returned to room temperature, and the reaction solution was then extracted with chloroform. The obtained organic layer was dried over magnesium sulfate and then concentrated under reduced pressure, so as to obtain the title compound (14.5 g).1H-NMR (400 MHz, CDCl3) delta (ppm): 2.49 (s, 3H), 2.60 (s, 3H), 12.8 (brs, 1H) |
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