Diisopentyl ether → diisoamyl ether DEAC

HRID 622468

Reaction equation

HRID 622468 reaction equation
[Cl-:1].[CH2:2]([Al+:4][CH2:5][CH3:6])[CH3:3].[CH2:7]([O:12][CH2:13][CH2:14][CH:15]([CH3:17])[CH3:16])[CH2:8][CH:9]([CH3:11])[CH3:10]>CCCCCC>[CH2:13]([O:12][CH2:7][CH2:8][CH:9]([CH3:11])[CH3:10])[CH2:14][CH:15]([CH3:16])[CH3:17].[Cl-:1].[CH2:2]([Al+:4][CH2:5][CH3:6])[CH3:3]

Participants

4

Reactant 2

HCID 10989Diisopentyl etherHCID 16686102Diethyl aluminum chloride

Product 1

HCID 131713250diisoamyl ether DEAC

Reagents, catalysts & solvents 1

HCID 8058HexaneSolvent

Procedure

n-Hexane (6 l), diethylaluminum monochloride (DEAC) (5.0 mols) and diisoamyl ether (12.0 mols) were mixed at 25° C. for 5 minutes, followed by reacting these at the same temperature for 5 minutes to obtain a reaction fluid (I) (the molar ratio of diisoamyl ether/DEAC:2.4). TiCl4 (40 mols) was introduced into a reactor equipped with a stirrer and purged with nitrogen and heated to 35° C., followed by dropwise adding thereto the total quantity of the above reaction fluid (I) over 180 minutes, thereafter keeping the mixture at the same temperature for 30 minutes, raising the temperature up to 75° C., further reacting it for one hour, cooling down to room temperature, removing the supernatant, and four times repeating a procedure of adding n-hexane (30 l) and removing by decantation to obtain a solid product (II) (1.9 Kg).

Workup

  1. customfor 5 minutes

Sources & evidence

ORD record
ord-0047674a4420405e9b27630c3eb1576e
Source dataset
uspto-grants-1988_09
Patent number
US04771103

Linked notes

Loading…