Compound preparation method
A compound and reactant technology, applied in the field of compound preparation, can solve problems such as difficult large-scale production, difficult purification of synthetic products, and high preparation costs
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Embodiment 1
[0048] Example 1: Preparation of the compound of formula (IV).
[0049] 1. The synthesis route is as follows:
[0050]
[0051] 2. Specific steps.
[0052] 1. A monoalkyl substitution reaction of 1,4,7,10-tetraazacyclododecane with N-Boc-bromoethylamine, including:
[0053] 1.1 Dissolve 1.7g of 1,4,7,10-tetraazacyclododecane in 20mL of chloroform to obtain solution A;
[0054] 1.2 At room temperature, add 1.34g of N-Boc-bromoethylamine to solution A and react for 18 hours to obtain reactant B;
[0055] 1.3 The reactant B is distilled off the solvent under reduced pressure to obtain the product C;
[0056] 1.4 The product C was purified by column chromatography with dry loading and eluent DCM / MeOH: 20 / 1, DCM / MeOH: 10 / 1 and DCM / MeOH: 5 / 1 containing 3% triethylamine 1 were eluted sequentially, and then concentrated by rotary evaporation and dried to obtain the compound of formula (I).
[0057] 2. Carry out nucleophilic substitution reaction with the compound of formula (I...
Embodiment 2
[0072] Example 2: Preparation of the compound of formula (IV).
[0073] One, synthetic approach is the same as embodiment 1.
[0074] 2. Specific steps.
[0075] 1. A monoalkyl substitution reaction of 1,4,7,10-tetraazacyclododecane with N-Boc-bromoethylamine, including:
[0076] 1.1 Dissolve 1.7g of 1,4,7,10-tetraazacyclododecane in 25mL of chloroform to obtain solution A;
[0077] 1.2 At room temperature, add 1.45g of N-Boc-bromoethylamine to solution A, and react for 20 hours to obtain reactant B;
[0078] 1.3 The reactant B is distilled off the solvent under reduced pressure to obtain the product C;
[0079] 1.4 The product C was purified by column chromatography with dry loading and eluent DCM / MeOH: 20 / 1, DCM / MeOH: 10 / 1 and DCM / MeOH: 5 / 1 containing 3% triethylamine 1 were eluted sequentially, and then concentrated by rotary evaporation and dried to obtain the compound of formula (I).
[0080] 2. Carry out nucleophilic substitution reaction with the compound of formul...
Embodiment 3
[0095] Example 3: Preparation of the compound of formula (IV).
[0096] One, synthetic approach is the same as embodiment 1.
[0097] 2. Specific steps.
[0098] 1. A monoalkyl substitution reaction of 1,4,7,10-tetraazacyclododecane with N-Boc-bromoethylamine, including:
[0099] 1.1 Dissolve 1.7g of 1,4,7,10-tetraazacyclododecane in 30mL of chloroform to obtain solution A;
[0100] 1.2 At room temperature, add 1.57g of N-Boc-bromoethylamine to solution A, and react for 24 hours to obtain reactant B;
[0101] 1.3 The reactant B is distilled off the solvent under reduced pressure to obtain the product C;
[0102] 1.4 The product C was purified by column chromatography with dry loading and eluent DCM / MeOH: 20 / 1, DCM / MeOH: 10 / 1 and DCM / MeOH: 5 / 1 containing 3% triethylamine 1 were eluted sequentially, and then concentrated by rotary evaporation and dried to obtain the compound of formula (I).
[0103] 2. Carry out nucleophilic substitution reaction with the compound of formul...
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