S-benzothiazol-2-yl 2-(2-amino-1,3-thiazol-4-yl)-2-(methoxyimino)thioacetate synthesis
- Product Name:S-benzothiazol-2-yl 2-(2-amino-1,3-thiazol-4-yl)-2-(methoxyimino)thioacetate
- CAS Number:94088-75-2
- Molecular formula:C13H10N4O2S3
- Molecular Weight:350.44
Yield:94088-75-2 97%
Reaction Conditions:
with pyridine;triethylamine;triethyl phosphite in dichloromethane;acetonitrile at 16.5 - 23; for 2 h;Temperature;Reagent/catalyst;
Steps:
1 The green process for synthesizing AE-active ester by microwave assisting comprises the following steps:
Add 30g of aminothiaoximoacidand 50g of DM to 350mL of dichloromethane-acetonitrile mixture at 21-23 °C.Add 7.2mL of triethylamine, 0.4mL of pyridine, cool down to 16.5-18 ° C, add 23mL of triethyl phosphite, add 1h,Using a microwave reactor, the microwave holding temperature was adjusted to 17 ° C, the microwave radiation power was 80 W, the irradiation time was 60 min, and the stirring speed was 100 rpm.Cool down to below 10 ° C, suction filtration to obtain a crude product. The crude product was soaked in 150 mL of methanol at 22-24 ° C for 1 h to obtain 50.8 g of purified AE-active ester.The yield was 97% and the purity was 99.1%.
References:
CN109053628,2018,A Location in patent:Paragraph 0030-0038
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