1-ETHYL-3-PYRROLIDINOL

1-ETHYL-3-PYRROLIDINOL Property

Boiling point:

59-61 °C1 mm Hg(lit.)

Density 

0.967 g/mL at 25 °C(lit.)

refractive index 

n20/D 1.467(lit.)

Flash point:

165 °F

storage temp. 

Sealed in dry,Room Temperature

form 

clear liquid

pka

14.83±0.20(Predicted)

color 

Colorless to Brown

CAS DataBase Reference

30727-14-1(CAS DataBase Reference)

Safety

Hazard Codes 

Xi

Risk Statements 

36/37/38

Safety Statements 

26-36/37/39

WGK Germany 

3

RTECS 

UY5685500

HS Code 

2933998090

Toxicity

mouse,LD50,intravenous,180mg/kg (180mg/kg),U.S. Army Armament Research & Development Command, Chemical Systems Laboratory, NIOSH Exchange Chemicals. Vol. NX#02177,

Hazard and Precautionary Statements (GHS)

Symbol(GHS)

Signal word

Warning

Hazard statements

H227Combustible liquid

H315Causes skin irritation

H319Causes serious eye irritation

H335May cause respiratory irritation

Precautionary statements

P210Keep away from heat/sparks/open flames/hot surfaces. — No smoking.

P261Avoid breathing dust/fume/gas/mist/vapours/spray.

P264Wash hands thoroughly after handling.

P264Wash skin thouroughly after handling.

P280Wear protective gloves/protective clothing/eye protection/face protection.

P305+P351+P338IF IN EYES: Rinse cautiously with water for several minutes. Remove contact lenses, if present and easy to do. Continuerinsing.

P370+P378In case of fire: Use … for extinction.

P403+P235Store in a well-ventilated place. Keep cool.

P501Dispose of contents/container to..…

1-ETHYL-3-PYRROLIDINOL Chemical Properties,Usage,Production

Synthesis

The present embodiment is a method for the preparation of 1-ethyl-3-pyrrolidinol, which was carried out as follows: 250 g of 40 wt% aqueous ethylamine solution was added to a 500 mL four-necked flask, cooled to 10 °C, and placed in an ice-water bath. Under stirring conditions, 102 g of 1,4-dichloro-2-butanol was added dropwise, and the temperature was controlled to be about 15 °C. After the dropwise addition was completed in about 15 min, the reaction system was transferred to a 500 mL autoclave, sealed, evacuated to a pressure of 1.0±0.1 MPa, heated to 120±2°C, stirred and reacted for about 10 h. The reaction was monitored by GC until the raw material disappeared. After the reaction was completed, cooled to room temperature, discharged the reaction material, added 110g of sodium hydroxide in batches, taking care to control the temperature below 50°C to release ethylamine gas and precipitate a white solid, and continued stirring for 1h. After filtration, the filtrate was layered, the upper organic phase was taken, 100mL of ethanol and 18g of anhydrous magnesium sulfate were added, and stirred for 2~3h. Filtered again, and the filtrate was concentrated under vacuum to obtain a yellow transparent The filtrate was again filtered and concentrated under vacuum to obtain a yellow transparent oily liquid, and finally 46.7 g of colorless and transparent 1-ethyl-3-pyrrolidinol was obtained by vacuum distillation with a yield of 64.8% and a purity of 99.3% (HPLC).

References

[1] Patent: CN106631956, 2017, A. Location in patent: Paragraph 0022; 0023; 0024; 0025; 0026; 0027