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s-1,3-Benzothiazol-2-yl benzenecarbothioate → 2,2-Bis{4-[2-benzoyloxy-3-(7,7,9,9-tetramethyl-1,4-dioxa-8-azaspiro[4.5]dec-8-yl)propoxy]cyclohexyl}propane
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | s-1,3-Benzothiazol-2-yl benzenecarbothioate | HCID 270394 | — |
| 反応物 | 2,2-Bis{4-[2-hydroxy-3-(7,7,9,9-tetramethyl-1,4-dioxa-8-azaspiro[4.5]dec-8-yl)propoxy]cyclohexyl}propane | HCID 20510600 | — |
| 溶媒 | Benzene | HCID 241 | — |
| 生成物 | 2,2-Bis{4-[2-benzoyloxy-3-(7,7,9,9-tetramethyl-1,4-dioxa-8-azaspiro[4.5]dec-8-yl)propoxy]cyclohexyl}propane | HCID 20510562 | — |
反応手順
1.5 g of 2,2-bis{4-[2-hydroxy-3-(7,7,9,9-tetramethyl-1,4-dioxa-8-azaspiro[4.5]dec-8-yl)propoxy]cyclohexyl}propane and 1.2 g of 2-benzoylthiobenzthiazole were refluxed in 30 ml of anhydrous benzene for 4.5 hours. After completion of the reaction, the reaction mixture was treated with an aqueous alkali and then extracted with benzene, giving crystals. The crystals were purified by column chromatography through silica gel eluted with a 4:1 by volume mixture of diethyl ether and ethyl acetate. The desired Compound No. 222 was obtained in the form of a white powder melting at 77°-79° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04371644 |
| 出典データセット | uspto-grants-1983_02 |
| ORD ID | ord-915f9cc3d87843bab679e9efbedb4fe3 |
| 出典メモ | uspto-grants-1983_02 |