Diethylamine → 2-methoxyethyldiethylamine

A solution prepared by mixing together 100 mL of diethylamine and 85 mL of 2-methoxyethyl chloride (both available from Kanto Chemical) was placed in an autoclave and reacted at 120° C. for 12 hours. The internal pressure during the reaction was 0.28 MPa (2.9 kgf/cm2). This yielded a mixture of deposited crystals and reaction solution to which was added, following the 12 hours of reaction, 200 mL of an aqueous solution prepared by dissolving 40 g of sodium hydroxide (Katayama Chemical Industries Co., Ltd.) in 200 mL of water. Each of the two divided organic phases that formed as a result was separated off with a separatory funnel and subjected twice to extraction with 250 mL of tetrahydrofuran (Wako Pure Chemical Industries, Ltd.). The separated organic phases were then combined and washed with a saturated saline solution, following which potassium carbonate (Wako Pure Chemical Industries) was added to remove water and vacuum filtration was carried out. The solvent in the resulting organic phase was distilled off in a rotary evaporator, after which the residue was subjected to normal-pressure distillation, yielding 21 g of 2-methoxyethyldiethylamine.

1. customA solution prepared
2. customreacted at 120° C. for 12 hours
3. customThis yielded
4. additiona mixture of deposited crystals and reaction solution to which
5. additionwas added
6. customprepared
7. customEach of the two divided organic phases that formed as a result
8. customwas separated off with a separatory funnel
9. extractionsubjected twice to extraction with 250 mL of tetrahydrofuran (Wako Pure Chemical Industries, Ltd.)
10. washwashed with a saturated saline solution
11. additionwas added
12. customto remove
13. filtrationwater and vacuum filtration
14. distillationThe solvent in the resulting organic phase was distilled off in a rotary evaporator
15. distillationafter which the residue was subjected to normal-pressure distillation

ORD record

ord-691f272e836f4be0b6cf9fd541a0c216

Source dataset

uspto-grants-2008_03

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07347954B2