ChemicalBook CAS DataBase List 1,1-DIPHENYL-2-PROPYN-1-OL

1,1-DIPHENYL-2-PROPYN-1-OL synthesis

13synthesis methods

Product Name:1,1-DIPHENYL-2-PROPYN-1-OL
CAS Number:3923-52-2
Molecular formula:C15H12O
Molecular Weight:208.26

119-61-9 Synthesis

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Yield:3923-52-2 99.2%

Reaction Conditions:

with sodium ethanolate in ethanol at 0 - 5; for 0.5 h;Inert atmosphere;Large scale;

Steps:

4 Example 1. Preparation of methylbutynol

General procedure: In a 10 L three-necked flask, 6 L of anhydrous methanol was added, and the mixture was shielded with nitrogen. Under cooling with ice water, 550 g of sodium metal (small) was slowly added.After all the sodium metal was dissolved, 1.5 L of acetone was added, and the mixture was uniformly stirred and cooled to below 0 °C. Slowly pass acetylene, The flow rate of the acetylene is controlled so that the reaction temperature is 0 to 5 °C. When the reaction is no longer exothermic, the reaction is complete. Then, a small amount of acetylene was introduced, and the closed micro-positive pressure (nitrogen balloon was not changed) was reacted for 0.5 hour. In another 20 L three-necked flask, 2.5 kg of ammonium chloride and 3 L of methanol were added.Under ice cooling, the reaction solution was poured into an ammonium chloride system to carry out a neutralization reaction. The neutralization reaction temperature was controlled to be less than 20 °C. After the neutralization is completed, it is filtered. The filtrate was first distilled with methanol, methanol was applied, and then the product methylbutynol was distilled under reduced pressure to obtain 1.69 kg. The product purity was 99.5%, and the yield was 99.1%.

References:

CN108863717,2018,A Location in patent:Paragraph 0036; 0037; 0038; 0043; 0044; 0045; 0046

119-61-9 Synthesis

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