6-BROMO-2-METHYL-2H-PHTHALAZIN-1-ONE synthesis
- Product Name:6-BROMO-2-METHYL-2H-PHTHALAZIN-1-ONE
- CAS Number:1234616-69-3
- Molecular formula:C9H7BrN2O
- Molecular Weight:239.07
75884-70-7
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74-88-4
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1234616-69-3
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$492.00/1g
Yield:1234616-69-3 86.6%
Reaction Conditions:
with sodium hydride in N,N-dimethyl-formamide at 0 - 20; for 72 h;Inert atmosphere;
Steps:
431.1 Step 1: 6-bromo-2-methylphthalazin-1(2H)-one
To a stirred mixture of 6-bromophthalazin-1(2H)-one (5 g,22.2 mmol)and NaH (1.1 g,60%wt,27.5 mmol)in DMF (50 mL) , was added methyl iodide (2.1 mL,33.3 mmol)at 0 under N 2 atmosphere. The resulting mixture was stirred for 3 days at room temperature under nitrogen atmosphere. The reaction was quenched with sat. aq. NH 4Cl solution and extracted with EA. The combined organic layers were washed with brine, dried over anhydrous Na 2SO 4. After filtration, the filtrate was concentrated under reduced pressure. The residue was purified by column chromatography (DCM/MeOH, 0-5%) to afford product (4.6 g, 86.6%) . [M+H] + = 239.1.
References:
WO2022/12622,2022,A1 Location in patent:Page/Page column 321-322
586-75-4
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$10.00/5g
1234616-69-3
13 suppliers
$492.00/1g