関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 1-Naphthyl Isothiocyanate | HCID 11080 | — |
| 反応物 | Sodium Azide | HCID 33557 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | HCID 178527985 | HCID 178527985 | 85% |
反応手順
To a solution of 1-naphthalenylisothiocyanate (500 mg, 2.7 mmol) in ethanol (150 mL) was added sodium azide (2.8 g, 43 mmol) and the mixture was heated to 79° C. for 2 hours. The reaction mixture was then cooled to room temperature, aqueous HCl solution (12N, 1.5 mL) added and the mixture concentrated. The resulting residue was diluted with ethyl acetate and extracted with aqueous NaOH solution (1N) and the aqueous layer acidified with aqueous HCl solution (12N) until a precipitate formed. The precipitate was collected and used in the next step without further purification (520 mg, 85% yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08372807B2 |
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| 出典データセット | uspto-grants-2013_02 |
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| ORD ID | ord-c8da1addf57740abb8024f26521d5f0c |
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| 出典メモ | uspto-grants-2013_02 |
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