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

In 50.0 ml of 1,2-dimethoxyethane (DME), 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 8.4 g of phosphorus oxychloride at 5° C. to a mixture of 20 ml of DME 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 160 ml of ice water to precipitate crystals. The resulting crystals were collected by filtration, washed with 200 ml of ice water and then stirred for 30 minutes in 120 ml of n-hexane. After filtration, the resulting crystals were dried under reduced pressure, whereby the title compound was obtained. Yield: 8.43 g (76.6%). Purity: 97.2%.

1. additionfollowed by the dropwise addition of a chlorinating reagent, which
2. customhad been prepared beforehand
3. customfor 30 minutes
4. customAfter they were reacted for 5 minutes
5. customto precipitate crystals
6. filtrationThe resulting crystals were collected by filtration
7. washwashed with 200 ml of ice water
8. filtrationAfter filtration
9. dry with materialthe resulting crystals were dried under reduced pressure, whereby the title compound
10. customwas obtained

ORDレコード

ord-0757c3bbfa1d443bb6f3447a86ec152b

出典データセット

uspto-grants-1995_06

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US05428173