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2,6-Lutidine → Benzo[d][1,2,3]thiadiazole-7-carbaldehyde
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2,6-Lutidine | HCID 7937 | — |
| 反応物 | 1,2,3-Benzothiadiazole-7-carbonyl chloride | HCID 18377607 | — |
| 触媒 | Palladium | HCID 23938 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | Benzo[d][1,2,3]thiadiazole-7-carbaldehyde | HCID 14835681 | — |
反応手順
99 g of benzo-1,2,3-thiadiazole-7-carboxylic acid chloride are dissolved in 1.2 l of ethyl acetate, the mixture is treated at 0°-5° C. with a solution of 58.7 g of 2,6-lutidine in 200 ml of tetrahydrofuran as well as 33 g of palladium/charcoal catalyst (5% Pd), and hydrogenated under low pressure (104Pa) with a further addition of a total of 57 g of palladium/charcoal catalyst and 500 ml of tetrahydrofuran in 5 portions. The catalyst is subsequently removed by filtration and washed with tetrahydrofuran, and the filtrate is evaporated. The residue is purified on silica gel (CH2Cl2) and gives the title compound of m.p. 134°-136° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05260423 |
| 出典データセット | uspto-grants-1993_11 |
| ORD ID | ord-d433502191674bf18c619faa0ceef992 |
| 出典メモ | uspto-grants-1993_11 |