Process for preparing 6-oxo-(6H)-dibenz-›C,E! ›1,2!-oxaphosphorins

• US 5,717,127 A
• Filed: 04/17/1996
• Issued: 02/10/1998
• Est. Priority Date: 04/24/1995
• Status: Expired due to Fees

• Current Assignee: Bayer AG
• Original Assignee: Bayer AG
• Inventors: Glock, Volker, Buysch, Hans-Josef
• Primary Examiner(s): Richter, Johann
• Assistant Examiner(s): AMBROSE, MICHAEL GEORGE
• Application Number:
  US08/633,609
• Time in Patent Office: 664 Days
• Field of Search: 558/82
• US Class Current: 558/82
• CPC Class Codes: C07F 9/65719 the ring phosphorus atom and, at least, one ring oxygen atom being part of a (thio)phosphonous acid derivative

Abstract

For the continuous preparation of 6-oxo-(6H)-dibenz- c,e! 1,2!-oxaphosphorins (ODOPs), 6-chloro-(6H)-dibenz- c,e! 1,2!-oxaphosphorins (CDOPs) are continuously reacted with at least the stochiometrically required amount of water at elevated temperature in a reaction section having little backmixing.

Claims

1. A process for preparing a 6-oxo-(6H)-dibenz- c,e! 1,2!-oxaphosphorin (ODOP) of the formula ##STR4## where R¹ to R⁶ are identical or different and are hydrogen, halogen, C₁ -C₄ -alkyl or C₁ -C₄ -alkoxy,

by reaction of an o-phenylphenol of the formula ##STR5## where R¹ to R⁶ are as defined above,

with phosphorus trichloride in the presence of a Lewis acid with elimination of hydrogen chloride at elevated temperature in the range from 70°

to 220°

C. in a 1st stage and hydrolysis of the product of the 1st stage in a 2nd stage, wherein, for the purposes of the hydrolysis, ab-chloro-(6H)-dibenz c,e!-oxaphosphorin and water in an at least stoichiometric molar ratio are fed continuously at elevated temperature into a reaction section having very little backmixing, the hydrolysis is carried out continuously along this reaction section at elevated temperature, the reaction products are discharged continuously at the end of the section and ODOP is optionally subjected to further treatment at elevated temperature.

2. The process of claim 1, wherein the o-phenylphenol used is one in which two of the radicals R¹ to R⁶ are hydrogen.

3. The process of claim 2, wherein the o-phenylphenol used is one in which four of the radicals R¹ to R⁶ are hydrogen.

4. The process of claim 3, wherein unsubstituted o-phenylphenol is used.

5. The process of claim 1, wherein a total amount of H₂ O of from 1 to 2 mol is used per tool of CDOP.

6. The process of claim 5, wherein a total amount of H₂ O of from 1 to 1.7 mol is used per mol of CDOP.

7. The process of claim 6, wherein a total amount of H₂ O of from 1 to 1.5 is used per mol of CDOP.

8. The process of claim 1, wherein the hydrolysis is carded out at a temperature of from 60°

to 250°

C.

9. The process of claim 8, wherein the hydrolysis is carried out at a temperature of from 80°

to 230°

C.

10. The process of claim 9, wherein the hydrolysis is carded out at a temperature of from 100°

to 220°

C.

11. The process of claim 10, wherein the hydrolysis is carried out at a temperature of from 130°

to 210°

C.

12. The process of claim 1, wherein both stages, but independently of one another, are carded out at pressures of from 0.5 to 50 bar.

13. The process of claim 12, wherein both stages, but independently of one another, are carded out at pressures of from 0.6 to 40 bar.

14. The process of claim 13, wherein both stages, but independently of one another, are carried out at pressures of from 0.8 to 30 bar.

15. The process of claim 1, wherein the finished reaction mixture after separating off HCl is subjected to treatment at elevated temperature in the range from 130°

to 250°

C.