関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | 1,3-Dioxan-5-ol, 2-phenyl- | HCID 74362 | — |
| 反応物 | Triphosgene | HCID 94429 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | HCID 58455273 | HCID 58455273 | — |
反応手順
Triphosgene (bis(trichloromethyl)carbonate (13.35 g, 45.0 mmol) was added under argon at room temperature to a solution of 1,3-O-benzylideneglycerol (18.02 g, 100.0 mmol) in dry CH2Cl2 (300 ml). The reaction mixture was cooled to −40° C. and a solution of pyridine (10.9 ml, 135.0 mmol) was added over 35 min under stirring. Upon completion of the addition the reaction mixture was stirred for 30 min at −40° C. Then it was allowed to warm to 0° C. over 60 min and subsequently warmed to rt over 3.5 h under stirring. The reaction product was used in the next step without any further purification
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08535655B2 |
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| 出典データセット | uspto-grants-2013_09 |
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| ORD ID | ord-88743db5226e4fbcacc170e4ad06550f |
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| 出典メモ | uspto-grants-2013_09 |
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