# US 5,705,677 A · Diphenyl oxalate-phenol adduct, process for producing the adduct and method of producing diphenyl oxalate from the adduct

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- Number: US 5,705,677 A
- Document ID: US5705677A
- Status: Granted
- Kind: A
- Application number: 08/757,070
- Filed: 1996-11-26
- Granted: 1998-01-06
- Earliest claimed: 1995-11-28
- Assignees: Ube Industries, Ltd.
- Inventors: Keigo Nishihira; Shuji Tanaka; Yuki Nishida; Hirofumi Ii; Satoru Fujitsu
- Web page: https://patentgrep.com/patent/US5705677A

## CPC

- C07C 69/017: Esters of hydroxy compounds having the esterified hydroxy group bound to a carbon atom of a six-membered aromatic ring
- C07C 69/36: Oxalic acid esters
- C07C: ACYCLIC OR CARBOCYCLIC COMPOUNDS

## Abstract

A novel crystalline adduct of diphenyl oxalate and phenol in a molar ratio of 1:2 and having a high purity is produced by melting a mixture containing diphenyl oxalate and phenol at a temperature of 100.degree. C. or more; cooling the melt to a temperature of less than 100.degree. C. to allow a resultant adduct of diphenyl oxalate and phenol in a molar ratio of 1:2 to crystallize and deposit from the melt; and collecting the crystalline adduct. Diphenyl oxalate with a high purity is produced by melting the crystalline adduct to dissociate it into diphenyl oxalate and phenol, and evaporating away the dissociated phenol from the melt to collect the dissociated diphenyl oxalate.

## Claims

### Claim 1

A process for producing a crystalline adduct of diphenyl oxalate and phenol, comprising the steps of:
melting a mixture containing diphenyl oxalate and phenol at a temperature of 100.degree. C. or more,
cooling the melt to a temperature of less than 100.degree. C. to allow a resultant adduct of diphenyl oxalate and phenol in molar ratio of 1:2 to crystallize and deposit from the melt; and
collecting the resultant crystallized diphenyl oxalate-phenol adduct.

### Claim 2 (depends on 1)

The process as claimed in claim 1, wherein the melt prepared in the melting step contains diphenyl oxalate in a content of 1 to 50% by weight based on the total weight of diphenyl oxalate and phenol.

### Claim 3 (depends on 1)

The process as claimed in claim 1, wherein the cooling is carried out at a temperature of 10.degree. C. to 95.degree. C.

### Claim 4 (depends on 1)

A method of producing diphenyl oxalate from the crystalline diphenyl oxalate-phenol adduct as claimed in claim 1, comprising the steps of:
melting a crystalline diphenyl oxalate-phenol adduct having a molar ratio of 1:2 to dissociate the adduct into diphenyl oxalate and phenol; and
evaporating away the dissociated phenol from the melt to collect the dissociated diphenyl oxalate.

### Claim 5 (depends on 4)

The method as claimed in claim 4, wherein the phenol-evaporation is carried out at a temperature of 100.degree. C. to 300.degree. C.

### Claim 6 (depends on 5)

The method as claimed in claim 5, wherein the phenol-evaporation temperature is from 190.degree. C. to 250.degree. C.

### Claim 7 (depends on 4)

The method as claimed in claim 4, wherein the phenol-evaporation is carried out under a reduced pressure of from 270 to 67,000 Pa.