関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Stannous chloride dihydrate | HCID 61436 | — |
| 反応物 | 4-Amino-2,3-dimethylbenzoic acid | HCID 2762777 | — |
| 反応物 | Sodium Nitrite | HCID 23668193 | — |
| 溶媒 | Hydrochloric Acid | HCID 313 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2,3-Dimethyl-4-hydrazinobenzoic acid hydrochloride | HCID 70244582 | 93.7% |
反応手順
A solution of 1.87 g of NaNO2 in 7 ml of water is added slowly to a solution, cooled to -5° C., of 4.5 g of 4-amino-2,3-dimethylbenzoic acid in 135 ml of concentrated HCl. After 2 hours of stirring at -5° C., a solution of 25 g of SnCl2.2H2O in 250 ml of concentrated HCl is added at -10° C., and the mixture is stirred for 30 minutes at -5° C. and then 2 hours at RT. The mixture is filtered, and the precipitate is washed with 5 ml of concentrated HCl and dried under a stream of dry nitrogen and then under vacuum to obtain 5.5 g of expected product.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05925661 |
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| 出典データセット | uspto-grants-1999_07 |
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| ORD ID | ord-32155afffc974c758ede7725d66a02ba |
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| 出典メモ | uspto-grants-1999_07 |
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