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ChemicalBook CAS DataBase List Dibutylurea

Dibutylurea synthesis

15synthesis methods
The reactions under CO2 pressured conditions were carried out in a stainless steel reactor (SUS 304, 30 mL, TVS-5 type). Thus, butylamine (2.9 g, 40 mmol), Ph3SbO (370 mg, 1.0 mmol), P4S10 (890 mg, 2.0 mmol), and benzene (20 mL) were charged into the reactor, and then CO2 was introduced at a pressure of 4.9 MPa (50 kg cm-2, ca. 65 mmol) at room temperature. The reactor was heated at 80 ℃ in a temperature-regulated incubator for 12 h. When a reaction temperature higher than 100 ℃ was necessary, an oil bath was used. After the heating, the reactor was cooled and carefully decompressed. The contents were treated with hot benzene (3×20 mL) and filtered to remove an insoluble residue containing the catalyst and phosphoric acid derivatives. The collected benzene solution was then concentrated to dryness in vacuo with cooling. Pure 1,3-dibutylurea was isolated by recrystallization from ligroin (yield 2.99 g, 88%).
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Yield: 88%

Reaction Conditions:

with manganese oxide;sodium carbonate in toluene for 10 h;Irradiation;

Steps:

3 Example 3
34.48 parts of carbon tetrabromide (content of 97.0%) were added to the reactor containing 85.00 parts of toluene, 14.78 parts of n-butylamine (content of 99.0%), 0.31 parts of trimanganese tetroxide (99.5%) and 10.88 parts of sodium carbonate (content 99.8%), under the xenon lamp as the light source, stir and react for 10 hours, then stand for layering. The upper layer is light yellow transparent liquid, and the lower layer is red and black oily bromine element. The upper layer solution is distilled and recovered Using toluene as a solvent, a yellow-brown solid product of 1,3-di-n-butylurea was obtained.

References:

CN112920089, 2021, A Location in patent:Paragraph 0045-0046; 0057

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