N-Boc-1,3-propanediamine synthesis
- Product Name:N-Boc-1,3-propanediamine
- CAS Number:75178-96-0
- Molecular formula:C8H18N2O2
- Molecular Weight:174.24
24424-99-5
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Yield:75178-96-0 100%
Reaction Conditions:
in dichloromethane at 0 - 20; for 3 h;Inert atmosphere;
Steps:
37 Preparation of Compound 101
In dichloromethane (30 mL), 1,3-diaminopropane (0.93 mL, 11.1 mmol) was dissolved, and di-t-butyl dicarbonate (0.84 mL, 3.7 mmol) was added thereto at 0°C under a nitrogen atmosphere. After the reaction solution was stirred at room temperature for 3 hours, brine (50 mL) was added to the reaction solution, the mixture was subjected to extraction using ethyl acetate (2 × 100 mL), and then the extract was dried over anhydrous sodium sulfate. After filtration, the reaction solution was filtered, then concentrated under reduced pressure, and purified by column chromatography to obtain Compound 101 (658 mg, 100% based on Boc2O). 1H-NMR (400 MHz, CDCl3) δ 4.88 (br s, 1H), 3.26-3.14 (m, 2H), 2.77 (t, J = 6.8 Hz, 2H), 1.66-1.57 (m, 2H), 1.44 (s, 9H), 1.32 (br, 2H).
References:
EP3604311,2020,A1 Location in patent:Paragraph 0244; 0245
129392-84-3
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