# US 5,352,782 A · Process for preparing crystalline .beta.-lactam monohydrate

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- Number: US 5,352,782 A
- Document ID: US5352782A
- Status: Granted
- Kind: A
- Application number: 08/071,552
- Filed: 1993-06-04
- Granted: 1994-10-04
- Earliest claimed: 1993-06-04
- Assignees: Eli Lilly and Company
- Inventors: Robert L. Nist; Marvin E. Wildfeuer
- Web page: https://patentgrep.com/patent/US5352782A

## CPC

- C07D 205/085: with a nitrogen atom directly attached in position 3
- C07D: HETEROCYCLIC COMPOUNDS (macromolecular compounds C08)

## Abstract

The invention provides a process for the preparation of the crystalline monohydrate form of the compound of the formula (I) ##STR1## which comprises the step of mixing a form of loracarbef, other than the crystalline monohydrate, such as the ethanol crystal, acetone crystal, crystalline dihydrate, acetonitrile crystal, methanol crystal, propanol crystal, ethyl acetate crystal, methylene chloride crystal, crystalline bis(DMF) and crystalline mono(DMF) form, in water at a temperature between about 30.degree. C. to about 60.degree. C., and preferably at a temperature between 40.degree. C. and 50.degree. C. Conversion may also be accomplished by exposing the loracarbef form to saturated steam at a temperature of between about 90.degree. to about 100.degree. C. Another aspect of the invention is the preparation of the above mentioned crystal forms by slurrying the bis(DMF) solvate form of the compound of formula (I) with the respective solvent.

## Claims

### Claim 1

A process for the preparation of the crystalline monohydrate form of the compound of the formula (I): ##STR4## which comprises the step of (a) mixing a form of the compound of formula (I), other than the crystalline monohydrate form, in water at a temperature between about 30.degree. to about 60.degree. C.; or
(b) exposing a form of the compound of formula (I), other than the crystalline monohydrate form, to saturated steam at a temperature of between about 90.degree. C. to about 100.degree. C.

### Claim 2 (depends on 1)

The process as recited in claim 1 wherein the water temperature is between 40.degree. C. and 50.degree. C.

### Claim 3 (depends on 1)

The process as recited in claim 1 wherein the form of loracarbef is selected from the ethanol crystal, acetone crystal, crystalline dihydrate, acetonitrile crystal, methanol crystal, propanol crystal, ethyl acelate crystal, methylene chloride crystal, crystalline bis(DMF) or crystalline mono(DMF) form.

### Claim 4 (depends on 3)

The process as recited in claim 3 wherein said form is ethanol crystal, acetone crystal, acetonitrile crystal, methanol crystal, propanol crystal, ethyl acetate crystal or methylene chloride crystal form.

### Claim 5 (depends on 4)

The process as recited in claim 4 further comprising the step of forming the solvent crystal form of the compound by slurrying the crystalline bis(DMF) solvate form of the compound with the respective solvent.

### Claim 6 (depends on 5)

The process as recited in claim 5 wherein said solvent is ethanol or acetone.

### Claim 7 (depends on 1)

The process as recited in claim 1 further comprising the step of drying the crystalline monohydrate.

### Claim 8 (depends on 1)

The process as recited in claim 1 further comprising the step of filtering the crystalline monohydrate.

### Claim 9

A process for the preparation of the crystalline monohydrate form of the compound of the formula (I): ##STR5## which comprises the step of mixing a form of the compound of formula (I), other than the crystalline monohydrate form, in water at a temperature between about 30.degree. to about 60.degree. C.