ChemicalBook CAS DataBase List METHYL 1-HYDROXY-1-CYCLOPROPANE CARBOXYLATE, 90

METHYL 1-HYDROXY-1-CYCLOPROPANE CARBOXYLATE, 90 synthesis

4synthesis methods

Product Name:METHYL 1-HYDROXY-1-CYCLOPROPANE CARBOXYLATE, 90
CAS Number:33689-29-1
Molecular formula:C5H8O3
Molecular Weight:116.12

72784-43-1 Synthesis

72784-43-1
85 suppliers
$55.00/250mg

METHYL 1-HYDROXY-1-CYCLOPROPANE CARBOXYLATE, 90

33689-29-1
104 suppliers
$16.00/1g

Yield:33689-29-1 75.5%

Reaction Conditions:

with sulfuric acid;sodium nitrite in water at 0;Reflux;

Steps:

1.1; 2.1 (1) Synthesis of Compound 2
Compound 1 (1200.0g, 10.4mol, 1.0eq) was dissolved in 12L aqueous sulfuric acid(Prepared by adding 98% concentrated sulfuric acid 0.57L to water, sulfuric acid molar equivalent is 1.0eq),The temperature of the ice bath was reduced to 0-5 ° C, and 3.5 L of sodium nitrite was added to the reaction solution(793.5g, 11.5mol, 1.1eq) aqueous solution, stirred at room temperature for 1 hour.Then add the above reaction dropwise to the refluxing 35L sulfuric acid aqueous solution B(Prepared by adding 98% concentrated sulfuric acid 0.57L to water, sulfuric acid molar equivalent is 1.0eq),After the dropwise addition is complete, stop heating and cool to room temperature. After the completion of the TLC detection reaction,Extract three times with ethyl acetate (3 * 12L), combine the organic phases, and dry over anhydrous magnesium sulfate,Filtration and concentration of the organic phase gave compound 2(910.8g, 22.1mmol), colorless oily liquid, yield 75.5%.

References:

Shanghai Tianze Bio-pharmaceutical Co., Ltd.;Li Jinfei CN110862311, 2020, A Location in patent:Paragraph 0034-0037; 0043-0045

FullText

17994-25-1 Synthesis