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

HRID 22474
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HRID 22474 반응식
[NH2:1][C:2]1[S:6][N:5]=[C:4](/[C:7](=[N:11]/[O:12][CH3:13])/[C:8](O)=[O:9])[N:3]=1.C(Cl)(=O)C([Cl:17])=O.CN(C)C=O>O1CCCC1>[NH2:1][C:2]1[S:6][N:5]=[C:4](/[C:7](=[N:11]/[O:12][CH3:13])/[C:8]([Cl:17])=[O:9])[N:3]=1
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참가 물질

5

반응물 3

HCID 6228DimethylformamideHCID 65578Oxalyl chlorideHCID 101304122-(5-Amino-1,2,4-thiadiazol-3-yl)-2-(methoxyimino)acetic acid

생성물 1

HCID 10198354(2Z)-2-(5-amino-1,2,4-thiadiazol-3-yl)-2-methoxyiminoacetyl chloride

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

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 6.97 g of oxalyl chloride at 5° C. to a mixture of 100 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 250 ml of ice water to precipitate crystals. The crystals were collected by filtration and washed with 100 ml of ice water. The resulting crystals were thereafter suspended in water and the suspension was adjusted to pH 4.0 with a 1M aqueous solution of sodium acetate. The resulting solution was extracted with 250 ml of ethyl acetate. The organic layer was dried over magnesium sulfate, followed by filtration. The filtrate was concentrated and, under reduced pressure, was then dried, whereby the title compound was obtained. Yield: 7.5 g (68.7%). Purity: 98.7 %.

후처리

  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 crystals were collected by filtration
  7. washwashed with 100 ml of ice water
  8. extractionThe resulting solution was extracted with 250 ml of ethyl acetate
  9. dry with materialThe organic layer was dried over magnesium sulfate
  10. filtrationfollowed by filtration
  11. concentrationThe filtrate was concentrated and, under reduced pressure
  12. customwas then dried

출처 및 근거

ORD 기록
ord-3ce216c8344a4ad0a3b0aeeb16824aef
출처 데이터셋
uspto-grants-1995_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05428173

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