ChemicalBook CAS DataBase List (Z)-3-Methylpent-2-en-4-yn-1-ol

(Z)-3-Methylpent-2-en-4-yn-1-ol synthesis

8synthesis methods

Product Name:(Z)-3-Methylpent-2-en-4-yn-1-ol
CAS Number:6153-05-5
Molecular formula:C6H8O
Molecular Weight:96.13

74915-98-3
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6153-05-5
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6153-06-6
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Yield:6153-05-5 86% ，6153-06-6 11%

Reaction Conditions:

with toluene-4-sulfonic acid in tetrahydrofuran; for 0.333333 h;Reflux;

Steps:

1.7-1.9; 2.7-2.8; 3.7-3.8; 4.7-4.8

7) Dissolve 3-methyl-3,5-dihydroxy-1-pentyne in a solvent to make a secondary solution; the solvent is toluene; the amount of the solvent is per gram of 3-methyl-3,5- Dihydroxy-1-pentyne was added 4ml; (8) add dehydration acid in the secondary solution, then adopt the reflux water separation device to carry out distillation dehydration; when the water stops being discharged from the water separation device, continue to distill 20min to complete the dehydration reaction, and the remaining material in the distillation device is dehydration material; dehydration; The acid is p-toluenesulfonic acid; the amount of dehydrated acid is added with 0.05 gram of dehydrated acid per gram of 3-methyl-3,5-dihydroxy-1-pentyne; (9) adding lye to the dehydrated material for neutralization, then adopting an oil-water separator for oil-water separation to separate the water phase and the remaining oil phase; the lye is an ammonia bicarbonate solution with a mass concentration of 0.5 to 5%, and the dosage is according to the lye The volume ratio to the solvent is 1:2; the main components of the oil phase are Z-3-methyl-2-penten-4-yn-1-ol and E-3-methyl-2-penten-4-yne -1-ol; wherein the mass content of Z-3-methyl-2-penten-4-yn-1-ol is 86%, E-3-methyl-2-penten-4-yn-1-ol The mass content of 11%; (10) adopt distiller to carry out distillation of oil phase, distillation temperature is lower than 100 , and the part separated out by distillation is intermediate 3-methyl-2-penten-4-yn-1-ol, and the remainder is distillation Residual liquid; when the mass percentage of intermediate 3-methyl-2-penten-4-yn-1-ol in the distillation residue is less than 0.3%, the distillation ends; intermediate 3-methyl-2-pentene- The purity of 4-yn-1-ol is 97.8% and the yield is 95%

References:

CN114315525,2022,A Location in patent:Paragraph 0064-0066; 0076-0077; 0086-0087; 0096-0097