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ChemicalBook CAS DataBase List 4-CHLORO-5-METHYLTHIENO[2,3-D]PYRIMIDINE
43088-67-1

4-CHLORO-5-METHYLTHIENO[2,3-D]PYRIMIDINE synthesis

3synthesis methods
-

Yield:43088-67-1 39%

Reaction Conditions:

with trichlorophosphate at 110; for 1 h;

Steps:

9.2

Step 2. Preparation of 4-chloro-5-methyl-thienor2.3-dlpyrimidine; The compound, 5-methyl-thieno[2,3-d]pyrimidin-4-ol, (1.4g, 8.42mmol) prepared in the step 1 was dissolved in phosphorusoxy chloride (5ml). Thereafter, the reaction mixture was stirred at 11O0C for 1 hour. After reaction, the reaction mixture was poured into ice water and chloroform, and washed with water and saturated sodium hydrogen carbonate aqueous solution. Combined organic layer was concentrated under reduced pressure. The residue was purified by recrystallization (n-hexane and ethyl acetate) to give 590mg (yield: 39%, yellow solid) of the target compound.[514] 1U NMR(400D, CDCI): δ 8.81 (s, IH), 7.24 (s, IH), 2.70 (s, 3H).

References:

WO2007/102679,2007,A1 Location in patent:Page/Page column 49

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