関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Citric Acid | HCID 311 | — |
| 反応物 | 1-Iodohexadecane | HCID 11007 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | Trihexadecyl citrate | HCID 6452032 | 83% |
反応手順
1,8-Diazabicyclo[5.4.0]undec-7-ene(1,5-5)(4.567 g, 30 mmol) was added at room temperature to a solution of citric acid (1.924 g, 10 mmol) in N,N-dimethylformamide (50 ml). 1-Iodohexadecane (10.570 g, 30 mmol) was added and the resulting mixture was stirred at 50° C. for 21 hours. The precipitated product was filtered off and washed with N,N-dimethylformamide and the crude product was purified by flash chromatography on silica gel using chlorform/hexane for elution. Yield: 83%. 1H-NMR (300 MHz, CDCl3): δ 088(t,9H), 1.26(m,78H), 1.60(m,6H), 2.84(q,4H), 4.07(t,4H), 4.13(s,1H), 4.20(t,2H). FAB-MS: 887.6(M+Na).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US06274120B1 |
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| 出典データセット | uspto-grants-2001_08 |
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| ORD ID | ord-ff189f389c904730b5eb2a8bd1af6d48 |
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| 出典メモ | uspto-grants-2001_08 |
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