Bogus Patent?

[jtryptamine]

Has anyone had success with this US patent #4,638,094?

http://patft.uspto.gov/netahtml/srchnum.htm

The patent claims "After the completion of the hydrolysis, the desired phenylacetone was quantitatively determined by a gas chromatographical analysis. The yield of the desired product was 85%". But Yield is more like 3-7% for me. I've tried nitrite oxidation of safrole, used both palladium chloride & mixed catalyst of palladium chloride and copper chloride, also tried both ethyl and methyl nitrate as oxidant. This has fail to produce the 85% claim numerous times. If anyone has had yields close to the claim let me know. I'm convinced this patent is bogus.

[Aurelius]

We can't help you without a DETAILED description of your reagents, where they came from (ie. purity), the catalyst source, ratios used, times, etc.  List everything.

[java]

This is the direct link to the patent in question in a PDF format.......java

Patent US4638094

[jtryptamine]

This post should have been written as a statement, not a question, my mistake. I have tried too many things to list. Diffrent reaction times, tempratures under vaccuum no vaccuum, diffrent sources of safrole. All chem. lab grade. Refer to ex.1 and 24 for more detail. This patent IS BOGUS and anyone who can thinks they can prove otherwise I would like to hear from you. I'm not interested in any thing but personal experience, all patent claims or internet refrences are not true! I must have tried over 50 times with diffrent variables and never came close to the claim. I guess the real question is why a japanese lab spent thousands of dollars on this false claim.

[Aurelius]

If it's really false, I don't think they spent the money.  Only enough to file the patent.  (in the U.S. that doesn't cost that much- not to file it anyway.)

[Rhodium]

A quick perusal of TFSE with your patent number gave the following:

Post 107768 (missing)

(smokemouth: "MDP2P with PdCl2 and MeONO, 73% - sunlight", Methods Discourse)

Post 107769 (missing)

(smokemouth: "Re: MDP2P with PdCl2 and MeONO, 73% - sunlight", Methods Discourse)

Post 108388 (missing)

(dormouse: "PdCl2 --> Pd(Ac)2. Help  -sunlight", Novel Discourse)

https://www.thevespiary.org/rhodium/Rhodium/chemistry/wacker.comments.txt

[Herr_Ovalmeister]

They claim priority from eight of their Japanese patent applications as you can see from the front of the US patent.  Did you check to see if they have a PCT?

[Herr_Ovalmeister]

Check out

Patent US3671590

which is listed on the front of

Patent US4638094

3671590 was assigned to Esso and is basically on the same process.
Also look at example 5, column 7, page 4 here:

Patent US3850990

No palladium!

[jtryptamine]

What I was trying to say is that I thought the patent was false. The link that Rodium gave supports this. Yes if you differ from the patent here and there it's successful, but if the patent is followed exactly, yields are extremely low.

  I was wondering why they filed it the way they did. I tried to contact the patent office via e-mail to see if the patent was just filed as auerulis suggested, but they just replied as to go to the patent office or get a lawyer. I think they assumed I wanted to file a patent.

  BTW has Herr_Ovalmeister had success w/the patent he stated, or just believing what he reads?

[Herr_Ovalmeister]

In your first post you wrote:

 also tried both ethyl and methyl nitrate as oxidant.

You need to use an alkyl nitrite not nitrate.

 But is a good dream. 100 cc of safrol single distilled ----->
 81 grams of MDP2P.
 It's my best one.

Post 107768 (missing)

(smokemouth: "MDP2P with PdCl2 and MeONO, 73% - sunlight", Methods Discourse)

 BTW has Herr_Ovalmeister had success w/the patent he stated, or just believing what he reads?

I don't believe what you write.

[jtryptamine]

I'm not going to argue with you if you don't believe me fine, that's good, one shouldn't believe everything he reads. But what I was getting at is don't say you have to do this or that if you don't have experience in the matter, try the patent as it's written then argue. Also this wasn't a how2 post, I know there are easier ways to MDP2P, like I said 3x I was wonderind why Ube lab. filed this.

[Herr_Ovalmeister]

Another important thing:
Methyl nitrate and ethyl nitrate are both explosive like nitroglycerine (glycerol trinitrate).  You can use methyl nitrite or ethyl nitrite in the process.  Read carefully and notice the difference in spelling.