関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | 1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride | HCID 2723939 | — |
| 反応物 | HCID 22719187 | HCID 22719187 | — |
| 反応物 | 8-(2-Furylmethoxy)-8-oxooctyl 2,5-dihydroxybenzoate | HCID 59005017 | — |
| 触媒 | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 8-(2-Furylmethoxy)-8-oxooctyl 2,5-bis[(4-{[6-(acryloyloxy)hexyl]oxy}benzoyl)oxy]benzoate | HCID 59005019 | — |
反応手順
A solution of N-(3-dimethylaminopropyl)-N′-ethylcarbodiimide hydrochloride (4.8 g) in dichloromethane (60 ml) was slowly added to a solution of 8-(2-furylmethoxy)-8-oxooctyl 2,5-dihydroxybenzoate (3.7 g), 4-(6-acryloylhexyloxy)benzoic acid (7.3 g) and 4-dimethylaminopyridine (0.6 g) in dichloromethane (150 ml) at 0° C. The mixture was stirred overnight at room temperature. The resulting solution was then added to water (600 ml) and extracted with dichloromethane (3×200 ml). The combined organic layers were washed with water (2×200 ml), dried over magnesium sulphate and filtered. The solvent removed in vacuum. The residue (10.4 g) was purified by column flash chromatography on silica gel using toluene/ethyl acetate (95:5) as eluent, to give 8-(2-furylmethoxy)-8-oxooctyl 2,5-bis[(4-{[6-(acryloyloxy)hexyl]oxy}benzoyl)oxy]benzoate.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08105662B2 |
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| 出典データセット | uspto-grants-2012_01 |
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| ORD ID | ord-c05dcc7cef6c47b8acfdd0b6b67beead |
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| 出典メモ | uspto-grants-2012_01 |
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