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1,2-Dibromoethane → 8-Methoxy-2,3-dihydrobenzo[b][1,4]dioxine-5-carboxylic Acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1,2-Dibromoethane | HCID 7839 | — |
| 反応物 | 2,3-Dihydroxy-4-methoxybenzoic acid | HCID 77534 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 8-Methoxy-2,3-dihydrobenzo[b][1,4]dioxine-5-carboxylic Acid | HCID 22734248 | 57% |
反応手順
171.5 g of 2,3-dihydroxy-4-methoxy benzoic acid, 515 cm3 of alcohol, 280 cm3 of soda lye and 175 g of ethylene bromide were introduced into a balloon flask provided with an agitator, a thermometer and an inlet pipe for nitrogen. The mixture was heated under reflux and then cooled and poured into 2.8 liters of water. The solution was filtered and treated with 85 cm3 of concentrated hydrochloric acid. The precipitate was dried off, washed and dried. After recrystallization in dimethylformamide, 110 g of 8-methoxy-1,4-benzodioxane-5-carboxylic acid were obtained (M.P.: 224°-226° C.; yield: 57%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04186135 |
| 出典データセット | uspto-grants-1980_01 |
| ORD ID | ord-e5b63fb7cc4340aeb14afe9575a4d2a1 |
| 出典メモ | uspto-grants-1980_01 |