METHOD FOR PURIFYING POLYETHYLENE GLYCOL HAVING ONE AMINO GROUP
First Claim
1. A method for purifying a polyethylene glycol compound having one amino group and having a total average molar number of ethylene oxide units added in a molecule thereof of 20 to 2300,the method comprising the following steps (A), (B) and (C):
- (A) a step of preparing an aqueous solution of the polyethylene glycol compound having one amino group, the solution having a pH of 1 to 5,(B) an extraction step of mixing the aqueous solution obtained in the step (A) with a mixed organic solvent at a temperature of 10°
C. or higher and 55°
C. or lower and causing layer separation into an organic layer and an aqueous layer, wherein a ratio of an organic solvent I is 25 to 65% by mass and a ratio of an organic solvent II is 75 to 35% by mass in the mixed organic solvent, the organic solvent I is selected from an aromatic hydrocarbon-based solvent having a total carbon number of 8 or less and an ester compound solvent containing no hetero atom and having a total carbon number of 5 or less, the organic solvent II is a halogenated hydrocarbon-based solvent, and a mixing ratio Y of the organic solvent I to the organic solvent II (organic solvent I/organic solvent II), temperature T (°
C.) at the mixing, and molecular weight M of the polyethylene glycol compound satisfy the following relationship;
1.9×
10−
6M+0.09≦
Y−
0.015T≦
−
1.4×
10−
6M+0.44, and(C) a step of recovering the polyethylene glycol compound from the aqueous layer.
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Abstract
A method for purifying a polyethylene glycol compound having one amino group, which includes (A) preparing an aqueous solution of the compound having a pH of 1 to 5, (B) an extracting step of mixing the aqueous solution with a mixed organic solvent to cause layer separation into organic and aqueous layers, wherein a ratio of an organic solvent I is 25 to 65% by mass and a ratio of an organic solvent II is 75 to 35% by mass, the organic solvent I is selected from an aromatic hydrocarbon and an ester, the organic solvent II is a halogenated hydrocarbon, and a mixing ratio Y of I to II, temperature T (° C.) at mixing, and molecular weight M of the compound satisfy the following relationship:
1.9×10−6M+0.09≦Y−0.015T≦−1.4×10−6M+0.44
and (C) recovering the compound from the aqueous layer.
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Citations
16 Claims
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1. A method for purifying a polyethylene glycol compound having one amino group and having a total average molar number of ethylene oxide units added in a molecule thereof of 20 to 2300,
the method comprising the following steps (A), (B) and (C): -
(A) a step of preparing an aqueous solution of the polyethylene glycol compound having one amino group, the solution having a pH of 1 to 5, (B) an extraction step of mixing the aqueous solution obtained in the step (A) with a mixed organic solvent at a temperature of 10°
C. or higher and 55°
C. or lower and causing layer separation into an organic layer and an aqueous layer, wherein a ratio of an organic solvent I is 25 to 65% by mass and a ratio of an organic solvent II is 75 to 35% by mass in the mixed organic solvent, the organic solvent I is selected from an aromatic hydrocarbon-based solvent having a total carbon number of 8 or less and an ester compound solvent containing no hetero atom and having a total carbon number of 5 or less, the organic solvent II is a halogenated hydrocarbon-based solvent, and a mixing ratio Y of the organic solvent I to the organic solvent II (organic solvent I/organic solvent II), temperature T (°
C.) at the mixing, and molecular weight M of the polyethylene glycol compound satisfy the following relationship;
1.9×
10−
6M+0.09≦
Y−
0.015T≦
−
1.4×
10−
6M+0.44, and (C) a step of recovering the polyethylene glycol compound from the aqueous layer. - View Dependent Claims (2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, 13, 14, 15, 16)
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Specification