4-AMINO-N-(6-CHLORO-5-METHOXY-4-PYRIMIDINYL)BENZENESULFONAMIDE synthesis
- Product Name:4-AMINO-N-(6-CHLORO-5-METHOXY-4-PYRIMIDINYL)BENZENESULFONAMIDE
- CAS Number:5018-23-5
- Molecular formula:C11H11ClN4O3S
- Molecular Weight:314.75
Yield:5018-23-5 85.3%
Reaction Conditions:
in N,N-dimethyl-formamide at 88 - 90; for 3 h;
Steps:
2 Example 2 Preparation of sulfadoxine intermediate condensate
In the reaction flask was added N, N- dimethylformamide 150g,Sulfacetamide sodium 110g was added with stirring,4,6-dichloro-5-methoxypyrimidine 50 g,Heated to 88 ~ 90 for 3 hours,DMF was depressurized to a temperature of 120 ° C, 200g of hot water above 90 ° C was added and dissolved. The diluted hydrochloric acid was adjusted to pH 7.0-8.0, cooled and filtered. The filtrate was adjusted to pH 3.8 with 5% diluted hydrochloric acid. The material was filtered and dried to give the sulfadoxine intermediate condensate 75g, yield 85.3%.Total impurities in HPLC: 1.75%, HPLC Max. Single impurity: 0.55%. See Figure 1 for details.
References:
CN104557735,2017,B Location in patent:Paragraph 0043; 0044