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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

反応式

関与物質

役割名称HCID仕込み量
反応物MethanolHCID 887—
反応物Lithium amideHCID 24532—
反応物1-(4-Hydroxy-2,2,6,6-tetramethylpiperidin-1-yl)ethan-1-oneHCID 14549312—
反応物N-(1-acetyl-2,2,6,6-tetramethyl-4-piperidinyl)glycine methyl esterHCID 20199419—
溶媒WaterHCID 962—
溶媒HeptaneHCID 8900—
生成物N-(1-acetyl-2,2,6,6-tetramethyl-4-piperidinyl)glycine(1-acetyl-2,2,6,6-tetramethyl-4-piperidinyl)esterHCID 1390792773.1%

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

DOI10.6084/m9.figshare.5104873.v1
特許番号US04670488
出典データセットuspto-grants-1987_06
ORD IDord-9d5162eb4def4d3f8226189749e3f025
出典メモuspto-grants-1987_06