반응 #50754

반응 방정식

N,N-dimethylformamide

2-(5-amino-1,2,4-thiadiazol-3-yl)-2(Z)-methoxyiminoacetic acid

trichloromethyl chloroformate

→

2-(5-amino-1,2,4-thiadiazol-3-yl)-2(Z)-methoxyiminoacetyl chloride

용매

THF

tetrahydrofuran

반응 조건

후처리

1. 1
   workup.ADDITIONfollowed by the dropwise addition of a chlorinating reagent, which
2. 2
   기타had been prepared beforehand
3. 3
   기타for 30 minutes
4. 4
   기타After they were reacted for 5 minutes
5. 5
   기타to precipitate crystals
6. 6
   여과The crystals were collected by filtration
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   세척washed with 100 ml of ice water
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   여과collected by filtration
9. 9
   여과After filtration
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    건조the resulting crystals were dried under reduced pressure, whereby the title compound
11. 11
    기타was obtained

실험 절차

In 30.0 ml of tetrahydrofuran (THF), 10.0 g of 2-(5-amino-1,2,4-thiadiazol-3-yl)-2(Z)-methoxyiminoacetic acid were stirred at -20° C., followed by the dropwise addition of a chlorinating reagent, which had been prepared beforehand by gradually adding 5.43 g of trichloromethyl chloroformate at 5° C. to a mixture of 80 ml of THF and 4.0 g of N,N-dimethylformamide (DMF) and then reacting them for 30 minutes. After they were reacted for 5 minutes, the reaction mixture was poured into 200 ml of ice water to precipitate crystals. The crystals were collected by filtration, washed with 100 ml of ice water, collected by filtration, and then stirred for 30 minutes in 100 ml of n-hexane. After filtration, the resulting crystals were dried under reduced pressure, whereby the title compound was obtained. Yield: 9.2 g (84.3%). Purity: 96.5%.

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