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Purification method for octahydro-1,1'-bi-2-naphtol (H8-BINOL)

A purification method, the technology of binaphthol, applied in the field of separation and purification of fine chemicals, can solve the problems of low solubility, large amount of recrystallization solvent, cumbersome operation process, etc., to reduce the amount of solvent used, and facilitate disassembly and cleaning , the effect of simple operation

Active Publication Date: 2019-09-27
XIAN MODERN CHEM RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the operation process of the prior art is cumbersome, and an additional recrystallization solvent is required, because 5,5',6,6',7,7',8,8'-octahydro-1,1'-bi-2-naphthalene Phenol is not very soluble in n-heptane, so the amount of recrystallization solvent required is also large

Method used

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  • Purification method for octahydro-1,1'-bi-2-naphtol (H8-BINOL)
  • Purification method for octahydro-1,1'-bi-2-naphtol (H8-BINOL)
  • Purification method for octahydro-1,1'-bi-2-naphtol (H8-BINOL)

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Effect test

Embodiment 1

[0027] Add 50g of silica gel powder to the ground casing in the purification device, raise the temperature of the heat transfer medium in the condensation tube in the purification device to 40°C, and prepare the 5,5',6,6',7,7 1500mL of ',8,8'-octahydro-1,1'-bi-2-naphthol reaction solution was passed into the purification device, purified by a silica gel powder bed to obtain a purified solution, and the solvent of the purified solution was evaporated completely, 5,5',6,6',7,7',8,8'-octahydro-1,1'-bi-2-naphthol with a content of 99.3% was obtained.

Embodiment 2

[0029]Add 50g of silica gel powder to the ground casing in the purification device, raise the temperature of the heat transfer medium in the condensation tube in the purification device to 60°C, and use binaphthol as raw material to prepare 5,5',6,6',7,7 1500mL of ',8,8'-octahydro-1,1'-bi-2-naphthol reaction solution was passed into the purification device, purified by a silica gel powder bed to obtain a purified solution, and the solvent of the purified solution was evaporated completely, 5,5',6,6',7,7',8,8'-octahydro-1,1'-bi-2-naphthol with a content of 99.7% was obtained.

Embodiment 3

[0031] Add 50g of silica gel powder to the ground casing in the purification device, raise the temperature of the heat conduction medium in the condensation tube in the purification device to 80°C, and use binaphthol as raw material to prepare 5,5',6,6',7,7 1500mL of ',8,8'-octahydro-1,1'-bi-2-naphthol reaction solution was passed into the purification device, purified by a silica gel powder bed to obtain a purified solution, and the solvent of the purified solution was evaporated completely, 5,5',6,6',7,7',8,8'-octahydro-1,1'-bi-2-naphthol with a content of 99.2% was obtained.

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Abstract

The method comprises the steps that the reaction liquid of the 5,5',6,6',7,7',8,8'-octahydro-1,1'-bi-2-naphtol (H8-BINOL) prepared by taking binaphthol as a raw material is introduced into a purification device for purification, exsolution is performed on purified liquid to obtain the 5,5',6,6',7,7',8,8'-octahydro-1,1'-bi-2-naphtol (H8-BINOL) with the content greater than or equal to 99%. The method comprises the steps that the reaction liquid of the (plus or minus)-5,5',6,6',7,7',8,8'-octahydro-1,1'-bi-2-naphtol prepared by taking binaphthol as a raw material is introduced into a purification device for purification, exsolution is performed on purified liquid to obtain the (plus or minus)-5,5',6,6',7,7',8,8'-octahydro-1,1'-bi-2-naphtol with the content of 99% or above. The purification device consists of a condenser pipe (1), ground joints (2), ground clamps (3) and a ground casing pipe (4) with open pores or pore channels, wherein the ground casing pipe is arranged in the condenser pipe for placing inorganic adsorbing materials. The method has the advantages of simple operation and high product purity.

Description

technical field [0001] The invention relates to a purification method of 5,5',6,6',7,7',8,8'-octahydro-1,1'-bi-2-naphthol, which belongs to the separation and purification of fine chemicals technology field. Background technique [0002] Asymmetric synthesis is an efficient method for the synthesis of chiral compounds, which has the advantages of chiral multiplication, high stereoselectivity, economy, and easy industrialization, but expensive chiral ligands delay the application of this method. Therefore, it is of great significance to screen out chiral ligands with high activity and low price. The binaphthyl skeleton is widely used in the synthesis of chiral ligands due to its steric hindrance, electron density, and dihedral angle. [0003] 5,5′,6,6′,7,7′,8,8′-octahydro-1,1′-binaphthol (hereinafter referred to as H 8 -BINOL) can achieve good chiral catalytic effect in asymmetric catalysis. Such as Albert S will H 8 When the complex of -BINOL and isopropyl titanate is u...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C37/82C07C37/00C07C39/14
CPCC07C37/82C07C37/00C07C2602/10C07C39/14
Inventor 陈涛毛明珍杨翠凤张晓光徐泽刚宁斌科
Owner XIAN MODERN CHEM RES INST
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