반응 #59261

반응 방정식

N′-(2-Cyclopropylethyl)hydrazinecarboxylic acid ethyl ester

NaOH

Oxalic acid

→

oxalate salt

수율 70.9%

2-Cyclopropylethyl-hydrazine oxalate salt

수율 70.9%

반응 조건

후처리

1. 1
   온도was cooled to room temperature
2. 2
   기타partitioned between brine and CH2Cl2
3. 3
   기타The organic layer was removed
4. 4
   건조dried over MgSO4
5. 5
   여과filtered
6. 6
   여과was filtered
7. 7
   기타dried in vacuo

실험 절차

N′-(2-Cyclopropylethyl)hydrazinecarboxylic acid ethyl ester (5a) (2.2 g, 12.6 mmol) was suspended in 7 mL of a 40% aqueous NaOH solution. The biphasic mixture was heated for 12 h at 120° C., upon which it was cooled to room temperature and partitioned between brine and CH2Cl2. The organic layer was removed, dried over MgSO4, and filtered. Oxalic acid (1.1 g, 12.6 mmol) was added to the filtrate, which after 12 h was filtered and dried in vacuo to yield 1.7 g (50%) of the oxalate salt (6a) as a white powder. 1H-NMR (400 MHz, D2O): 3.13 (t, 2H, J=7.2 Hz); 1.46 (q, 2H, J=7.2 Hz); 0.61 (m, 1H); 0.1 (d, 2H); 0.39 (m, 2H); 0.01 (m, 2H) ppm.

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