CN105294731A - Synthesis of N-biotinyl-N ,-Boc-1, 6-hexanediamine - Google Patents

Abstract

The invention discloses a synthetic method of N-biotin acyl-N'-Boc-1, 6-hexamethylenediamine. The synthetic method comprises the following steps: respectively adding biotin, HOBT and EDC hydrochloride into DMF at the room temperature, then, adding N'-Boc-1, 6-hexamethylenediamine, stirring at the room temperature overnight, spin-drying the DMF, adding methyl alcohol for separating out plenty of white solids, filtering, drying to obtain a crude product, and purifying, so as to obtain the N-biotin acyl-N'-Boc-1, 6-hexamethylenediamine. The N-biotin acyl-N'-Boc-1, 6-hexamethylenediamine synthesized by the invention is high in yield, good in crystallization effect and high in purity, and provides a high-purity standard sample or a sample for subsequent chemical and biological experiments.

Description

N-vitamin H acyl group-N ,the synthetic method of-Boc-1,6-hexanediamine

Technical field

The invention belongs to field of compound preparation, especially a kind of N-vitamin H acyl group-N'-Boc-1, the synthetic method of 6-hexanediamine.

Background technology

At present, because Bioexperiment makes new breakthroughs, make us in treatment and find in the process of the cause of disease, means are more, result is more accurate, property pharmaceutical requirements is also increased gradually so for the various disease for the treatment of, therefore, the various compound with New function is developed a large amount of, the whole world all has in searching the new compound resisting various difficult and complicated cases, in the process so developed at these new compounds, the compound of numerous new textures and new configuration can be produced, and then find useful in the new compound that these are numerous, there is the molecule for the treatment of use, therefore developing new compound is one and important process.

Summary of the invention

The object of the present invention is to provide a kind of N-vitamin H acyl group-N'-Boc-1, the synthetic method of 6-hexanediamine, synthesis step of the present invention is simple, finished product yield is high, foreign matter content is low.

The object of the invention is to be achieved through the following technical solutions:

A kind of N-vitamin H acyl group-N'-Boc-1, the synthetic method of 6-hexanediamine, step is as follows:

Respectively vitamin H and HOBT and EDC hydrochloride are joined in DMF under room temperature, then add N'-Boc-1,6-hexanediamine, stirred overnight at room temperature; be spin-dried for DMF, add methyl alcohol and separate out a large amount of white solid, filter; dry to obtain thick product, purifying obtains N-vitamin H acyl group-N'-Boc-1,6-hexanediamine.

And, described vitamin H: HOBT:EDC hydrochloride: the mol ratio of N'-Boc-1,6-hexanediamine is: 8:1:1:1.

Advantage of the present invention and positively effect are:

1, the N-vitamin H acyl group-N'-Boc-1 of the present invention's synthesis, the productive rate of 6-hexanediamine is high, and crystallization effect is good, and purity is high, for follow-up chemistry and Bioexperiment provide highly purified standard specimen or sample.

2, the invention provides N-vitamin H acyl group-N'-Boc-1, the synthesis condition in the building-up process of 6-hexanediamine, raw material, and the nuclear-magnetism figure of synthesis after product, for the analysis and identification of product each in building-up process provides detailed support.

Accompanying drawing explanation

Fig. 1 is N-vitamin H acyl group-N'-Boc-1, the nuclear-magnetism figure of 6-hexanediamine.

Embodiment

Below in conjunction with embodiment, the present invention is further described, and following embodiment is illustrative, is not determinate, can not limit protection scope of the present invention with following embodiment.

Vitamin H _ domestic market is bought

HOBT_ domestic market is bought

EDC hydrochloride _ domestic market is bought

Triethylamine _ purchase

Synthetic route of the present invention is as follows:

A kind of N-vitamin H acyl group-N'-Boc-1, the synthetic method of 6-hexanediamine, step is as follows:

Under room temperature, respectively by vitamin H (13.7g, 0.056mol) and HOBT (9.9g, 0.07mol) join in 300mlDMF with EDC hydrochloride (14.0g, 0.07mol), then add compound 2 (N'-Boc-1,6-hexanediamine) (15.8g, 0.07mol), stirred overnight at room temperature, is spin-dried for DMF, add methyl alcohol and separate out a large amount of white solid, filter, dry to obtain thick product 16.0g, purifying obtains 14.0g productive rate 67.1%.

Claims (2)

1. a N-vitamin H acyl group-N'-Boc-1, the synthetic method of 6-hexanediamine, is characterized in that: step is as follows:

Respectively vitamin H and HOBT and EDC hydrochloride are joined in DMF under room temperature, then add N'-Boc-1,6-hexanediamine, stirred overnight at room temperature; be spin-dried for DMF, add methyl alcohol and separate out a large amount of white solid, filter; dry to obtain thick product, purifying obtains N-vitamin H acyl group-N'-Boc-1,6-hexanediamine.

2. N-vitamin H acyl group-N'-Boc-1 according to claim 1, the synthetic method of 6-hexanediamine, is characterized in that: described vitamin H: HOBT:EDC hydrochloride: the mol ratio of N'-Boc-1,6-hexanediamine is: 8:1:1:1.