(4-Nitrophenyl)methyl 3-oxobutanoate synthesis
- Product Name:(4-Nitrophenyl)methyl 3-oxobutanoate
- CAS Number:61312-84-3
- Molecular formula:C11H11NO5
- Molecular Weight:237.21
Yield:61312-84-3 97%
Reaction Conditions:
with triethylamine in dichloromethane at 0 - 20; for 3 h;
Steps:
2 Example 2; Synthesis of 6-methyl-2-thioxo-l,2,3,4-tetrahydro-pyrimidine-5-carboxylicacid 4-nitro-benzyl ester (7)
4-Nitrobenzyl alcohol (1.53 g, 10 mmol) was introduced into a round bottomedflask, and dichloromethane (10 mNo. ) was added thereto. After the solution was cooledusing an ice bath, diketene (1.26 g, 15 mmol) was slowly added, and triethyknine(0.14 m-6 , 1 mmol) was added. This solution was warmed to room temperature, stirredfor 3 hours, and water (10 m-6 ) was added. The organic kyer was dried over MgSOand distilled under reduced pressure to give 4-nitrobenzyl acetoacetate (2.30 g,Yield=97%). The resulting 4-nitrobenzyl acetoacelate was reacted according to thesame procedure as Example 1 to give the title compound in the yield of 68% (2.09 g).1 H NMR(CDC1): 5 8.25(d, 2H), 7.53(s, 1H), 7.5l(d, 2H), 6.57(s, 1H), 5.27(s,32H), 4.21(s, 2H), 2.54(s, 3H)MS(M+1): 308
References:
WO2004/111013,2004,A1 Location in patent:Page 39-40
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