5-Methyl-1H-benzotriazole synthesis
- Product Name:5-Methyl-1H-benzotriazole
- CAS Number:136-85-6
- Molecular formula:C7H7N3
- Molecular Weight:133.15
63186-18-5
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Yield:136-85-6 93%
Reaction Conditions:
with iodine;aluminium in acetonitrile at 80; for 18 h;
Steps:
General Procedure C
General procedure: A mixture of iodine (0.212 g, 1.65 mmol), aluminum (0.052 g) and 13 (0.137 g, 0.5 mmol) in MeCN (10 mL) was stirred for 18 h at 80 °C in an oil bath. After quenching with dilute HCl (2 M, 5 mL), the mixture was extracted with ethyl acetate (50 mL × 3). The organic phases were combined, washed with saturated aqueous Na2S2O3 (5 mL) and then dried over MgSO4. After filtration, the solvents were removed using a rotary evaporator, and the residue was purified by column chromatography (petroleum ether/ethyl acetate 3:1, v/v) to afford 3 as an off-white solid. Yield: 0.055 g (92%).
References:
Dong, Bingqian;Liu, Yunfeng;Yang, Pengtao;Sang, Dayong;Tian, Juan;Li, Li;Long, Sihui [Tetrahedron Letters,2022,vol. 103,art. no. 153965] Location in patent:supporting information
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