関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetic Anhydride | HCID 7918 | — |
| 反応物 | 6,12,18-Tris(benzyloxy)-7,13-dioxo-6,12,18-triazaoctadecanenitrile | HCID 9986266 | — |
| 溶媒 | Pyridine | HCID 1049 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 6,12,18-Tris(benzyloxy)-7,13,19-trioxo-6,12,18-triazaeicosanenitrile | HCID 10100838 | 60% |
反応手順
Acetic anhydride (8 mL) was slowly added to a solution of (8) (1.25 g, 2.03 mmol) in pyridine (50 mL) and CH2Cl2 (30 mL) which had been cooled to 0° C. Stirring was continued at 0° C. for 30 minutes and then at room temperature overnight. Solvents were removed under high vacuum, and the residue was dissolved in CHCl3 (120 mL), followed by washing with 0.5N HCl (2×40 mL) and saturated NaHCO3 (2×40 mL). After solvent removal, the crude oil was purified by silica gel column chromatography, eluting with 3:1 EtOAc/hexane, to furnish 0.8 g (60%) of (9) as an oil: NMR δ 1.40-1.80 (m, 12 H), 2.05 (s, 3 H), 2.20-2.50 (m, 6 H), 3.40-3.73 (m, 6 H), 4.75 (s, 6 H) , 7.32 (s, 15 H). Anal. (C38H48N4O6) C, H, N.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05322961 |
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| 出典データセット | uspto-grants-1994_06 |
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| ORD ID | ord-215dcef00ec74818b619f710d9eaf4cb |
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| 出典メモ | uspto-grants-1994_06 |
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