PCE (Eticyclidine) Synthesis Procedure

[mxtlrr_chem]

PCE is a dissociative that produces dissociative, anesthetic and hallucinogenic effects.

Reagents:

- Anhydrous Ethylamine
- Cyclohexanone
- Potassium Hydroxide
- Lithium Metal
- Bromobenzene
- Ether
- Dilute HCl
- Sodium Hydroxide
- Water

Procedure:

100g anhydrous ethylamine is mixed with 220g cyclohexanone. Keep for 16 hours, then shake with solid Potassium Hydroxide. The lower oil layer contains N-cyclohexylidenethylamine, which is the intermediate. It should be decanted off. Next, phenyllithium is prepared by slowly adding 11g of lithium metal to 76mL bromobenzene in 500mL ether. This was added to 11g of the intermediate in 500mL water, with stirring and cooling to keep temperature at 0C. Mixture should be heated to reflux with stirring for 1 hour, then decomposed by addition of water.

The ether layer is seperated, washed with water, and extracted with dilute HCl. The acid layer is basified with Sodium Hydroxide and extracted back into organic solvent. The solvent should be evaporated, to yield N-ethyl-1-phenylcyclohexylamine (Eticyclidine/PCE) freebase.

To purify PCE, distillation should be done en vacuo.

 

[mxtlrr_chem]

If anything is ambigious, this may clear it up. Found at the Rhodium Chemistry Archive:

N-(cyclohexylidene)ethylamine Synthesis​

A mixture of concentrated anhydrous ethylamine (100g) and 220g cyclohexanone is allowed to sit for 16 hours. The reaction mixture shaken thorougly with solid KOH. Oil layer removed via decantation. It can be used crudely, or purified via vacuum distillation (but not required)

(1-phenylcyclohexyl)ethylamine (Eticyclidine) from the Intermediate​

A solution of phenyllithium is prepared from 11.2g lithium and 76mL of bromobenzene in 500mL ether. It is added dropwise at 0°C to a solution of 51g of the intermediate in 500mL ether. After addition is complete, mixture should be stirred for 1 hour. Water is to be added to decompose it. Ether layer is to be removed, washed with water and dried. Ether evaporated. Residue left behind yielding Eticyclidine (bp: 104-108C @ 2mmHg).

Purification can be done via vacuum distillation.

Eticyclidine HCl from Freebase​

The method above yields Eticyclidine freebase. If you want the HCl salt, dissolve freebase in excess of IPA solution of HCl(g), precipitating salt with ether and recrystallizing the product, which is obtained from ether-IPA mixture. (mp: 236-237C)