반응 #55513

ord-5176bc7b717446ac88b809a2854aef31

반응 방정식

CCCC=O
butyraldehyde
CCCC=O
Formula IV
CCCC=O
butyraldehyde
NC1CCCCC1
cyclohexylamine
NC1CCCCC1
Formula III
NC1CCCCC1
cyclohexylamine
O=S(=O)([O-])[O-].[Na+].[Na+]
sodium sulfate
CCCC=C1CCCCC1N
1-BUTYLIDENE CYCLOHEXYLAMINE
수율 86.0%

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타The product was decanted from the salt water slurry
  2. 2
    건조dried by addition of further 10 g of anhydrous sodium sulfate
  3. 3
    여과filtered
  4. 4
    workup.DISTILLATIONdistilled

실험 절차

At 0° C., 16.3 g (20 mL, 0.23 mol) of butyraldehyde (Formula IV) was added dropwise to 21.7 g (25 mL, 0.22 mol) of cyclohexylamine (Formula III). After 1 h, 6 g of anhydrous sodium sulfate was added and the mixture stirred for 5 h. The product was decanted from the salt water slurry, dried by addition of further 10 g of anhydrous sodium sulfate, filtered and distilled. Characteristics of the product: bp 88° C. (20 mm); yield 86%; NMR (CDCl3, δ): 1.0 (3H, t) 1.1-2.1 (12H), 2.3 (2H, g), 3.0 (1H, m), 7.8 (1H, t).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04220774uspto-grants-1980_09