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Methyl iodide → [4-[(Z)-C-methylsulfanyl-N-(trimethylsilylmethyl)carbonimidoyl]naphthalen-1-yl]methyl acetate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methyl iodide | HCID 6328 | — |
| 反応物 | Potassium tert-butoxide | HCID 23665647 | — |
| 反応物 | (4{[(Trimethylsilyl)methyl]carbamothioyl}naphthalen-1-yl)methyl acetate | HCID 58092092 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 溶媒 | tert-Butyl methyl ether | HCID 15413 | — |
| 生成物 | [4-[(Z)-C-methylsulfanyl-N-(trimethylsilylmethyl)carbonimidoyl]naphthalen-1-yl]methyl acetate | HCID 58092085 | 88.1% |
反応手順
To a mixed solution of methyl iodide (0.60 g) and (4{[(trimethylsilyl)methyl]carbamothioyl}naphthalen-1-yl)methyl acetate (1.2 g) in THF (30 ml) was added potassium t-butoxide (0.45 g) gradually, and the mixture was stirred for 20 minutes at the same temperature. The mixture was diluted with t-butyl methyl ether and washed with water and a saturated aqueous brine, subsequently dried over magnesium sulfate. After filtering the reaction mixture, the solvent was distilled off under reduced pressure, to obtain {4-[(Z)-(methylsulfanyl){[(trimethylsilyl)methyl]imino}methyl]naphthalen-1-yl}methyl acetate (1.1 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08304371B2 |
| 出典データセット | uspto-grants-2012_11 |
| ORD ID | ord-2d953f5932fc46c2a8ae6d97f8d737cd |
| 出典メモ | uspto-grants-2012_11 |