関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 4-tert-Butylbenzoic acid | HCID 7403 | — |
| 反応物 | 4-Methylmorpholine | HCID 7972 | — |
| 反応物 | Hydrazine | HCID 9321 | — |
| 反応物 | Isobutyl chloroformate | HCID 62365 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | Benzoic acid, 4-(1,1-dimethylethyl)-, hydrazide | HCID 123513 | — |
反応手順
A solution of 4-tert-butyl benzoic acid (0.2 g, 1.2 mmol in 10 mL of dry THF) cooled to 0° C. and treated with N-methyl-morpholine (1.6 mL, 14.6 mmol) as well as isobutyl chloroformate (1.7 mL, 1.3 mmol). Then the mixture was stirred for 10 minutes at 0° C. After hydrazine (0.6 g, 3.6 mmol) was added to the reaction mixture, it was stirred 3 hours at 25° C. The reaction was then diluted with ethyl acetate (100 mL), washed with saturated sodium bicarbonate solution as well as brine, and concentrated in vacuum. The crude material was chromatographed on silica gel eluting with hexanes/ethyl acetate=2:1 to give 4-tert-butyl-benzoic acid hydrazide.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06809119B2 |
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| 出典データセット | uspto-grants-2004_10 |
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| ORD ID | ord-f8af978295af440990998aaf3a31624f |
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| 出典メモ | uspto-grants-2004_10 |
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