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HRID 703529作成日:2026年10月26日
1,3-Benzodioxole-5-carboxylic acid → 1,3-Benzodioxole-5-carboxamide, N-((4-(2-(1-pyrrolidinyl)ethoxy)phenyl)methyl)-
https://huagongshe.com/reaction/703529
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1,3-Benzodioxole-5-carboxylic acid | HCID 7196 | — |
| 反応物 | Thionyl Chloride | HCID 24386 | — |
| 反応物 | 1,3-Benzodioxole-5-carbonyl chloride | HCID 2734749 | — |
| 反応物 | (4-(2-(Pyrrolidin-1-yl)ethoxy)phenyl)methanamine | HCID 14425929 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 生成物 | 1,3-Benzodioxole-5-carboxamide, N-((4-(2-(1-pyrrolidinyl)ethoxy)phenyl)methyl)- | HCID 3078816 | 89.7% |
反応手順
To a cooled solution of 20.0 g of 4-[2-(1-pyrrolidinyl)ethoxy]benzylamine in 30 ml of chloroform was added 17.7 g of 3,4-methylenedioxybenzoyl chloride (which was prepared with 15.9 g of piperonylic acid and 65.3 g of thionyl chloride in the usual manner). The mixture was stirred at room temperature for 20 minutes and the solvent was evaporated. 150 ml of water was added to the residue and the mixture was washed with ethyl acetate. The aqueous layer was made alkaline with potassium carbonate and was extracted with ethyl acetate. The extract was washed with water, dried, and evaporated. The residue was washed with isopropyl ether to give 30.0 g of colorless crystals, which were recrystallized from ethyl acetate as colorless needles, m.p. 93.5°-94.5° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04983633 |
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| 出典データセット | uspto-grants-1991_01 |
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| ORD ID | ord-bc3aa1fa71ee41219775f90b89013820 |
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| 出典メモ | uspto-grants-1991_01 |
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