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ChemicalBook CAS DataBase List 1-(Tetrahydro-2-furoyl)piperazine
63074-07-7

1-(Tetrahydro-2-furoyl)piperazine synthesis

3synthesis methods
-

Yield:63074-07-7 93%

Reaction Conditions:

in chloroform

Steps:

1 The preparation of N-(tetrahydrofuran-2-carbonyl) piperazine (Compound 3)
Example 1 The preparation of N-(tetrahydrofuran-2-carbonyl) piperazine (Compound 3) In a 100 ml round-bottom flask, tetrahydrofuran-2-carboxylic acid (3.48 grams, 30 mmole), piperazine (5.16 grams, 60 mmole) and 1,1,1,3,3,3-hexamethyldisilazane (4.83 grams, 30 mmole) were added, stirred under a nitrogen atmosphere and heated to 110° C. After 5 hours, the completion of the reaction was detected by thin-layer chromatography (TLC). After cooling to room temperature, the product was dissolved in chloroform, washed with a sodium hydrogen carbonate solution once and with water once. The organic layer was dried with anhydrous sodium sulfate, filtered, and applied suction to obtain 5.13 grams of Compound 3. Yield:: 93%. Compound 3: 1H NMR (CDCl3) δ 1.87-1.91 (m, 1 H), 1.93-2.07 (m, 2 H), 2.22-2.27 (m, 1 H), 2.45 (s, 1 H, NH), 2.85-2.91 (m4 H), 3.48-3.57 (m, 2 H), 3.60-3.69 (m, 2 H), 3.86-3.90 (m, 1 H), 3.93-3.99 (m, 1 H), 4.61 (dd, J=7.3, 5.4 Hz, 1 H); 13C NMR (CDCl3) δ 25.6 (t), 28.4 (t), 43.0 (t), 45.8 (t), 46.2 (t), 46.6 (t), 68.9 (t), 75.6 (d), 169.8 (s)

References:

Development Center for Biotechnology US6313293, 2001, B1

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