ChemicalBook CAS DataBase List 4-CHLORO-2-METHYL-5,6,7,8-TETRAHYDRO[1]BENZOTHIENO[2,3-D]PYRIMIDINE

4-CHLORO-2-METHYL-5,6,7,8-TETRAHYDRO[1]BENZOTHIENO[2,3-D]PYRIMIDINE synthesis

4synthesis methods

Product Name:4-CHLORO-2-METHYL-5,6,7,8-TETRAHYDRO[1]BENZOTHIENO[2,3-D]PYRIMIDINE
CAS Number:81765-97-1
Molecular formula:C11H11ClN2S
Molecular Weight:238.74

2-methyl-5,6,7,8-tetrahydrobenzo[4,5]thieno[2,3-d]pyrimidin-4(3H)-one

19819-15-9
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4-CHLORO-2-METHYL-5,6,7,8-TETRAHYDRO[1]BENZOTHIENO[2,3-D]PYRIMIDINE

81765-97-1
40 suppliers
$44.00/250mg

Yield:81765-97-1 97%

Reaction Conditions:

with trichlorophosphate at 110; for 3 h;

Steps:

3 Intermediate 4

Intermediate 3 (0.82 mmol) and 5 mL of POCl₃were added into a 100 mL evaporating flask. The reaction solution was refluxed under stirring at 110° C. for 3 h, then cooled to room temperature and evaporated to dryness by rotary evaporation under reduced pressure. The residue was dissolved in an appropriate amount of ethyl acetate and adjusted to be alkaline by adding a saturated aqueous NaHCO₃solution. Then the mixture was extracted with ethyl acetate, washed with a saturated NaCl aqueous solution, and the organic layer was evaporated to dryness by rotary evaporation to obtain an Intermediate 4 (white solid, 97% yield), which was directly put into next reaction without purification.

References:

US2022/227782,2022,A1 Location in patent:Paragraph 0059

19819-15-9
7 suppliers
inquiry

81765-97-1
40 suppliers
$44.00/250mg

References

4506-71-2 Synthesis