関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethanol | HCID 702 | — |
| 反応物 | p-Toluenesulfonic acid monohydrate | HCID 521998 | — |
| 反応物 | tris(2,4-bis(N,N-bis(2-t-butyldimethylsilyloxyethyl)sulfamoyl)phenyl)bismuthine | HCID 10606600 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | Tris(2,4-bis(N,N-bis(2-hydroxyethyl)sulfamoyl)phenyl)bismuthine | HCID 10844129 | 79.5% |
反応手順
13.59 g of the tris(2,4-bis(N,N-bis(2-t-butyldimethylsilyloxyethyl)sulfamoyl)phenyl)bismuthine preparation prepared in Example 5 was dissolved in a mixed solvent containing 13.6 ml of ethanol and 27 ml of dichloromethane, and 0.272 g of p-toluenesulfonic acid monohydrate was added thereto. The mixture was refluxed under heating at 50° C. for 6 hours, and then cooled to room temperature. The crystals were collected by filtration, washed with 29.5 ml of dichloromethane and dried. As a result, 5.54 g of the title compound was obtained as crystals with a melting point of 110°-113° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05730953 |
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| 出典データセット | uspto-grants-1998_03 |
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| ORD ID | ord-39d007a1ceb040768775ffb5002a1d9e |
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| 出典メモ | uspto-grants-1998_03 |
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