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HRID 577195作成日:2026年10月25日

Triethylamine → HCID 178429437、化合物

https://huagongshe.com/reaction/577195

反応式

関与物質

役割名称HCID仕込み量
反応物TriethylamineHCID 8471—
反応物Phosphorus tribromideHCID 24614—
反応物2,4-Dimethyl-3-pyridinemethanolHCID 10329351—
反応物HCID 178429541HCID 178429541—
溶媒DichloromethaneHCID 6344—
生成物HCID 178429437HCID 17842943764%

反応手順

(2,4-dimethylpyridin-3-yl)methanol was dissolved in dichloromethane (100 mL). Tribromophosphane (1.5 mL, 16 mmol) was added slowly. After 2 hours, the mixture was evaporated to dryness. The crude solid was dissolved in cold ethanol (100 mL), and 6-methyl-2-sulfanylpyrimidin-4-ol (1.13 g, 8.0 mmol) and triethylamine (4.5 mL, 32 mmol) were added. The resulting mixture was stirred at room temperature for 3 hours. The solvent was evaporated, and the crude solid was washed with THF (200 mL). After evaporation of solvent, the crude was purified by CombiFlash (0-6% MeOH in DCM) to provide 2-{[(2,4-dimethylpyridin-3-yl)methyl]sulfanyl}-6-methylpyrimidin-4-ol (2.5 g, 64% yield); 1H NMR (500 MHz, DMSO-d6): δ 2.23 (s, 3H), 2.68 (s, 3H), 2.84 (s, 3H), 4.62 (s, 2H), 6.05 (br, 1H), 7.71 (s, 1H), 8.62 (s, 1H); M+ 232.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US09040538B2
出典データセットuspto-grants-2015_05
ORD IDord-24bd45339ce04bd4967a1437bf2ff7b0
出典メモuspto-grants-2015_05