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HRID 652207作成日:2026年10月25日
Methanol → N-(1-acetyl-2,2,6,6-tetramethyl-4-piperidinyl)glycine(1-acetyl-2,2,6,6-tetramethyl-4-piperidinyl)ester
https://huagongshe.com/reaction/652207
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | Lithium amide | HCID 24532 | — |
| 反応物 | 1-(4-Hydroxy-2,2,6,6-tetramethylpiperidin-1-yl)ethan-1-one | HCID 14549312 | — |
| 反応物 | N-(1-acetyl-2,2,6,6-tetramethyl-4-piperidinyl)glycine methyl ester | HCID 20199419 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Heptane | HCID 8900 | — |
| 生成物 | N-(1-acetyl-2,2,6,6-tetramethyl-4-piperidinyl)glycine(1-acetyl-2,2,6,6-tetramethyl-4-piperidinyl)ester | HCID 13907927 | 73.1% |
反応手順
To a four-necked flask equipped with a thermometer, a stirrer and a Deanstark trap were added 27 g (0.1 mole) of N-(1-acetyl-2,2,6,6-tetramethyl-4-piperidinyl)glycine methyl ester, 21.9 g (0.11 mole) of 1-acetyl-2,2,6,6-tetramethyl-4-piperidinol, 0.23 g of lithium amide and 100 g of heptane. The temperature was raised with stirring, and reaction was carried out at 98° to 105° C. for 6 hours, during which methanol was removed from the reaction system by means of the Deanstark trap. After completion of the reaction, the reaction solution was cooled, and water was added thereto to dissolve the product in the heptane layer. The heptane layer was separated and concentrated by removing heptane by distillation. The residue was purified by column chromatographic separation to obtain 32 g of N-(1-acetyl-2,2,6,6-tetramethyl-4-piperidinyl)glycine(1-acetyl-2,2,6,6-tetramethyl-4-piperidinyl)ester as a pale yellow liquid. Yield, 73% based on N-(1-acetyl-2,2,6,6-tetramethyl-4-piperidinyl)-glycine methyl ester.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04670488 |
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| 出典データセット | uspto-grants-1987_06 |
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| ORD ID | ord-9d5162eb4def4d3f8226189749e3f025 |
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| 出典メモ | uspto-grants-1987_06 |
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