반응 #1063402

반응 방정식

4-methoxy-2-methylsulfonyl-6-trifluoromethylpyrimidine

n-butyllithium

O-methylhydroxylammonium chloride

water

→

product

수율 43.1%

2-(N-Methoxyamino)-4-methoxy-6-trifluoromethylpyrimidine

수율 43.1%

용매

n-hexane

tetrahydrofuran

반응 조건

후처리

1. 1
   workup.STIRRINGStirring
2. 2
   workup.WAITwas carried out for 1 hour at 25° C.
3. 3
   기타the organic phase was separated off
4. 4
   세척washed with water
5. 5
   기타dried
6. 6
   기타Removal of the solvent
7. 7
   기타gave an oily, slightly impure product, which
8. 8
   기타could be crystallized in pentane at -78° C

실험 절차

66.6 g of a 1.6 molar solution of n-butyllithium (0.156 mol) in n-hexane were added dropwise to a solution of 6.5 g of O-methylhydroxylammonium chloride (78 mmol) in 200 ml of tetrahydrofuran at -10° C. Stirring was carried out for 10 minutes at -10° C., and 20 g of 4-methoxy-2-methylsulfonyl-6-trifluoromethylpyrimidine (78 mmol) were added to the cloudy solution. Stirring was carried out for 1 hour at 25° C., the reaction batch was introduced into 200 ml of water, and the organic phase was separated off, washed with water and dried. Removal of the solvent gave an oily, slightly impure product, which could be crystallized in pentane at -78° C. 7.5 g of the product (43% of theory) were obtained as colorless crystals of melting point. 44°-46° C.

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