関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Chloro(diphenyl)silane | HCID 74206 | — |
| 反応物 | indium(III)chloride | HCID 159675 | — |
| 反応物 | 2-Benzyl-1,2,3,3a,7,7a-hexahydro-4-thia-2-aza-cyclopenta[alpha]pentalen-7-ol | HCID 131727050 | — |
| 溶媒 | 1,1-Dichloroethane | HCID 6365 | — |
| 生成物 | 2-Benzyl-1,2,3,3a,7,7a-hexahydro-4-thia-2-aza-cyclopenta[alpha]pentalene | HCID 131727049 | 57% |
反応手順
Indiumtrichloride (973 mg, 4.40 mmol) and chlorodiphenylsilane (2888 mg, 13.20 mmol) were added to a solution of the product from step f) (1192 mg, 4.40 mmol) in 20 mL of dichloroethane. The reaction mixture was heated at 60° C. overnight and then was cooled to room temperature and quenched with saturated NaHCO3 (50 ml). The reaction mixture was extracted with ethylacetate (2×50 mL). The combined organic extracts were washed with brine (50 ml), dried with MgSO4 and solvent evaporated in vacuo to afford the subtitle compound (638 mg, yield: 57%) that was used without further purification. MS calculated C16H17NS +H: 256, observed: 256.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07981919B2 |
|---|
| 出典データセット | uspto-grants-2011_07 |
|---|
| ORD ID | ord-c317cc8e23e144c0bf1594cabcb4b564 |
|---|
| 出典メモ | uspto-grants-2011_07 |
|---|