関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Stannous chloride dihydrate | HCID 61436 | — |
| 反応物 | 3-Amino-4-methylbenzoic acid | HCID 75568 | — |
| 反応物 | Sodium Nitrite | HCID 23668193 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 溶媒 | Hydrochloric Acid | HCID 313 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 3-Hydrazino-4-methylbenzoic acid hydrochloride | HCID 56777508 | — |
反応手順
A solution of 2.74 g of NaNO2 in 28 ml of water is added over 30 minutes to a solution, cooled to -5° C., of 5 g of 3-amino-4-methylbenzoic acid in 120 ml of concentrated HCl and 40 ml AcOH, and the mixture is left stirring for 1 hour 20 minutes at 0° C. After cooling to -10° C., a solution of 27.6 g of SnCl2.2H2O in 28 ml of concentrated HCl is added slowly. After stirring for 1 hour at RT, filtration, washing of the precipitate with 5 ml of 1N HCl and drying over P2O5 under vacuum, 6.15 g of the expected product are obtained.
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-7974467ab6f44f649dc5acb3e3908eac |
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| 出典メモ | uspto-grants-1999_07 |
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