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3-Methoxyphenylhydrazine hydrochloride → Methyl 3-[6-methoxy-3-(t-butylthio) indol-2-yl]-2,2-dimethylpropanoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 3-Methoxyphenylhydrazine hydrochloride | HCID 2723940 | — |
| 反応物 | Methyl 5-t-butylthio-2,2-dimethyl-4-oxopentanoate | HCID 14980531 | — |
| 溶媒 | tert-Butanol | HCID 6386 | — |
| 生成物 | Methyl 3-[6-methoxy-3-(t-butylthio) indol-2-yl]-2,2-dimethylpropanoate | HCID 53636575 | — |
反応手順
A mixture of 4.2 g of 3-methoxyphenylhydrazine hydrochloride and 4.9 g of methyl 5-(t-butylthio)-2,2-dimethyl-4-oxopentanoate in 100 mL of t-butanol was refluxed for 18 hours. The mixture was cooled to R.T., and evaporated to dryness. The residue was suspended in ether (150 ml) and stirred for 30 min. The salts were filtered and the filtrate evaporated to dryness to give a residue which was chromatographed on flash silica gel using as eluant ethyl acetate:toluene (1:99) to isolate the title compound as the most polar product; m.p. 133° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05272145 |
| 出典データセット | uspto-grants-1993_12 |
| ORD ID | ord-e997d33143774de09203f9999fd673d1 |
| 出典メモ | uspto-grants-1993_12 |