ChemicalBook CAS DataBase List TETRAMETHYLENE FORMAL

TETRAMETHYLENE FORMAL synthesis

6synthesis methods

Product Name:TETRAMETHYLENE FORMAL
CAS Number:505-65-7
Molecular formula:C5H10O2
Molecular Weight:102.13

67-56-1 Synthesis

67-56-1
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110-63-4 Synthesis

110-63-4
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$24.80/250g

505-65-7
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Yield:505-65-7 55%

Reaction Conditions:

with iron(III) chloride hexahydrate;sodium nitrite at 50; for 24 h;UV-irradiation;

Steps:

Photocatalytic synthesis of 1,3-dioxacyclanes. General procedure.

General procedure: The synthesis of cyclic acetals was performed on a photocatalytic installation Photo Catalytic Reactor Lelesil Innovative Systems with a quartz reactor of 250 mL capacity (Strohmeier photoreactor equipped with a magnetic stirrer). In the flask of the reactor was charged 6.3 mmol (1.70 g) of FeCl₃·6H₂O, 6.3 mmol (0.44 g) of sodium nitrite, and 500 mmol of primary alcohol (20 mL of methanol 1b, 30 mL of ethanol 2b), and the reaction mixture was stirred till the formation of a homogeneous solution (nitrogen oxides liberation occurred). Then 500 mmol of an appropriate diol was charged (30 g of ethylene glycol 1a, 45 g of 1,4-butanediol 2a, 52 g of 1,5-pentanediol 3a). The reactor was attached to the installation in keeping with the instruction of the producer. The radiation source is a mercury lamp of medium pressure of the power 250 W. The radiation spectral composition by energy is as follows: 48% of UV range, 43% of visible range, 9% of IR range. Spectral interval: 186-1368 nm. The light beam reached the reaction system passing through a water layer kept at a controlled temperature (20-50°C). Photoactivation time: 6-24 h. On completing the reaction the product was extracted in ethyl ether. The upper organic layer was separated on a separatory funnel, dried with anhydrous sodium sulfate, after distilling off ethyl ether the residue was subjected tofractional distillation.

References:

Makhmutov [Russian Journal of Organic Chemistry,2018,vol. 54,# 11,p. 1710 - 1714][Zh. Org. Khim.,2018,vol. 54,# 11,p. 1695 - 1698,4]

50-00-0 Synthesis