تفاعل #42842

معادلة التفاعل

ammonium chloride

4,6-dichloro-5-methylpyrimidine

sodium hydride

2-butyn-1-ol

→

4-chloro-6-(2-butynyloxy)-5-methylpyrimidine

المردود 91.2%

المذيبات

tetrahydrofuran

tetrahydrofuran

tetrahydrofuran

ظروف التفاعل

المعالجة

1. 1
   workup.STIRRINGstirred for 2 hours
2. 2
   استخلاصthe mixture was extracted with tert-butyl methyl ether three times
3. 3
   غسيلThe organic layers were washed with water
4. 4
   تجفيفdried over anhydrous magnesium sulfate
5. 5
   تركيزconcentrated

الإجراء التجريبي

0.32 g of sodium hydride (60% oil suspension) was suspended in 12 ml of tetrahydrofuran. 2 ml of tetrahydrofuran solution of 0.43 g of 2-butyn-1-ol was added dropwise at room temperature therein slowly, and the mixture was stirred for 20 minutes. Into the mixture was added dropwise 2 ml of tetrahydrofuran solution of 1 g of 4,6-dichloro-5-methylpyrimidine at 0° C. slowly, and stirred for 2 hours. The reaction mixture was poured into a saturated ammonium chloride aqueous solution, and the mixture was extracted with tert-butyl methyl ether three times. The organic layers were washed with water, dried over anhydrous magnesium sulfate and concentrated. The residue was subjected to silica gel column chromatography to obtain 1.1 g of 4-chloro-6-(2-butynyloxy)-5-methylpyrimidine.

المصدر