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HRID 60720作成日:2026年10月25日
Tris(trimethylsilyl)silane → [(3aS,5S,6aS)-2,2-dimethyl-3a,5,6,6a-tetrahydrofuro[2,3-d][1,3]dioxol-5-yl]methoxy-tert-butyl-diphenyl-silane
https://huagongshe.com/reaction/60720
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Tris(trimethylsilyl)silane | HCID 123134 | — |
| 反応物 | [(3aS,5R,6aS)-5-[[tert-butyl(diphenyl)silyl]oxymethyl]-2,2-dimethyl-3a,5,6,6a-tetrahydrofuro[2,3-d][1,3]dioxol-6-yl]oxy-phenoxy-methanethione | HCID 131737103 | — |
| 触媒 | Azobisisobutyronitrile | HCID 6547 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | [(3aS,5S,6aS)-2,2-dimethyl-3a,5,6,6a-tetrahydrofuro[2,3-d][1,3]dioxol-5-yl]methoxy-tert-butyl-diphenyl-silane | HCID 72707693 | 88.9% |
反応手順
To a solution of [(3aS,5R,6aS)-5-[[tert-butyl(diphenyl)silyl]oxymethyl]-2,2-dimethyl-3a,5,6,6a-tetrahydrofuro[2,3-d][1,3]dioxol-6-yl]oxy-phenoxy-methanethione (compound 25c, 17 g, 30 mmol) in toluene (150 mL) was added tri(trimethylsilyl)silane(16.4 g, 66 mmol) and azodiisobutyronitrile (98 mg, 0.6 mmol), the mixture was heated at 130° C. under nitrogen for 3 hours. After the reaction was completed, the reaction was concentrated in vacuo and the residue was purified by column chromatography on silica gel (eluting with 1:10 EtOAc in petroleum ether) to afford 11 g of [(3aS,5S,6aS)-2,2-dimethyl-3a,5,6,6a-tetrahydrofuro[2,3-d][1,3]dioxol-5-yl]methoxy-tert-butyl-diphenyl-silane (compound 25d).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09441008B2 |
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| 出典データセット | uspto-grants-2016_09 |
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| ORD ID | ord-dc5c38134d9d4bc38045b9f9864eade3 |
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| 出典メモ | uspto-grants-2016_09 |
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