反応 #623306

反応方程式

product

3-Benzyloxy-7-methyl-4-oxo-4H-pyrido[1,2-α]pyrimidine-2-carboxylic acid

3-methylbenzoyl hydrazine

1-hydroxybenzotriazole

1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride

→

desired compound

収率 53.0%

3-Methyl-benzoic acid N′-(3-benzyloxy-7-methyl-4-oxo-4H-pyrido[1,2-α]pyrimidine-2-carbonyl)-hydrazide

収率 53.0%

溶媒

tetrahydrofuran

反応条件

後処理

1. 1
   その他After 12 h the reaction solution was quenched with water (20 mL)
2. 2
   抽出extracted with ethyl acetate
3. 3
   洗浄The extract was washed with 2N aqueous hydrochloric acid (20 mL), 2N aqueous sodium hydroxide (20 mL)
4. 4
   乾燥dried (Na2SO4)
5. 5
   濃縮concentrated in vacuo

実験手順

To a solution of the product from Example 8.2 (200 mg, 0.644 mmol) in tetrahydrofuran (10 mL), was added 3-methylbenzoyl hydrazine (94.8 mg, 0.632 mmol), 1-hydroxybenzotriazole (6.98 mg, 0.0576 mmol) and 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (98 mg, 0.632 mmol) successively at room temperature. After 12 h the reaction solution was quenched with water (20 mL) and extracted with ethyl acetate. The extract was washed with 2N aqueous hydrochloric acid (20 mL), 2N aqueous sodium hydroxide (20 mL) dried (Na2SO4) and concentrated in vacuo to afford the desired compound (53%).

出典