I guess what I'm really wondering about is the stochiometry of this reaction. In other write-ups of the bayer-williger I can't seem to find this enormous amounts of GAA. Can somebody help me with the rationale? I'm really close to trying this one out, but the amount of GAA is problematic.
Excess acts as a solvent for the reaction. In terms of accessibility, try to use food vinegar concentrate.
No proble
No problem finding 60% concentration in large amounts. Would that suffice, or would I need to dehydrate it first?
I guess what I'm really wondering about is the stochiometry of this reaction. In other write-ups of the bayer-williger I can't seem to find this enormous amounts of GAA. Can somebody help me with the rationale? I'm really close to trying this one out, but the amount of GAA is problematic.
View attachment 1386
Langkah 1. 3-metil-4-fenil-3-buten-2-satu.
1. Campur 1000 g benzaldehida dan 1000 ml MEK, diaduk dan didinginkan pada 0 *C.
2. Gas HCl digelembungkan secara perlahan melalui campuran selama 1,5 jam.
3. Larutan diaduk selama 1,5 jam pada suhu kamar.
4. Ditambahkan air, dan larutan diekstraksi dengan kloroform, kemudian dicuci dengan larutan natrium bikarbonat dan dikeringkan (Na2SO4).
5. Pelarut dihilangkan di bawah vakum tinggi dan 3-metil-4-fenil-3-buten-2-satu didistilasi di bawah vakum (bp.76-78 *C). Hasil: 1000 gram.
View attachment 1387
Langkah 2. 2-Asetoksi-1-fenil-1-propena.
1. Produk dari Langkah 1, 10.000 ml asam asetat glasial dan 1300 g 50% H2O2 diaduk dan dipanaskan pada suhu 55 *C selama 23 jam.
2. Setelah itu ditambahkan air 10000 ml air.
3. Diekstraksi dengan 5000 ml kloroform.
4. Pelarut dihilangkan di bawah vakum untuk menghasilkan 800 g 2-Asetoksi-1-fenil-1-propena.
View attachment 1388
Langkah 3. 1-fenil-2-propanon.
1. Produk untuk Langkah 2 dan 600 g natrium hidroksida dalam 2500 ml air diaduk pada 50 °C selama 12 jam.
2. Larutan diekstraksi dengan 1000 ml kloroform, dikeringkan (Na2SO4) dan pelarut dihilangkan di bawah vakum. Hasil: 650 gram.
What would you suggest using if chloroform is not available?
I would say DCM, but I might be wrong
You also easily make chloroform by reacting cold 0* C bleach with acetone in stoechiometric amounts with a small 10% ish molar excess of bleach.Nilered has a video.
Sorry dir the Noob question i am Not a chemist.....View attachment 1386
Step 1. 3-methyl-4-phenyl-3-buten-2-one.
1. Mixed 1000 g benzaldehyde and 1000 ml MEK, stirring and chilled at 0 *C.
2. HCl gas was bubbled slowly through a mixture 1.5 hours.
3. The solution was stirred for 1.5 hours at room temperature.
4. Water was added, and the solution extracted with chloroform, then washed with sodium bicarbonate solution and dried (Na2SO4).
5. Solvent was removed under high vacuum and 3-methyl-4-phenyl-3-buten-2-one was distilled under vacuum (bp.76-78 *C). Yield: 1000 g.
View attachment 1387
William DampierView attachment 1386
Step 1. 3-methyl-4-phenyl-3-buten-2-one.
1. Mixed 1000 g benzaldehyde and 1000 ml MEK, stirring and chilled at 0 *C.
2. HCl gas was bubbled slowly through a mixture 1.5 hours.
3. The solution was stirred for 1.5 hours at room temperature.
4. Water was added, and the solution extracted with chloroform, then washed with sodium bicarbonate solution and dried (Na2SO4).
5. Solvent was removed under high vacuum and 3-methyl-4-phenyl-3-buten-2-one was distilled under vacuum (bp.76-78 *C). Yield: 1000 g.
View attachment 1387
Step 2. 2-Acetoxy-1-phenyl-1-propene.
1. Product from Step 1, 10000 ml glacial acetic acid and 1300 g 50% H2O2 was stirring and heated at 55 *C for 23 hours.
2. After this time water added 10000 ml water.
3. Extracted with 5000 ml chloroform.
4. Solvent removed under vaccum to yield 800 g of 2-Acetoxy-1-phenyl-1-propene.
View attachment 1388
Step 3. 1-phenyl-2-propanone.
1. Product for Step 2 and 600 g sodium hydroxide in 2500 ml water was stirred at 50 °C 12 hours.
2. Solution extracted with 1000 ml chloroform, dried (Na2SO4) and the solvent removed under vacuum. Yield: 650 g.
tic acid and 1300 g 50% H2O2 was stirring and heated at 55 *C for 23 hours.
2. After this time water added 10000 ml water.
3. Extracted with 5000 ml chloroform.
4. Solvent removed under vaccum to yield 800 g of 2-Acetoxy-1-phenyl-1-propene.
View attachment 1388
Step 3. 1-phenyl-2-propanone.
1. Product for Step 2 and 600 g sodium hydroxide in 2500 ml water was stirred at 50 °C 12 hours.
2. Solution extracted with 1000 ml chloroform, dried (Na2SO4) and the solvent removed under vacuum. Yield: 650 g.
HCl gas is bubbled slowly through the mixture for a 1.5 h.
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