Phosphorus pentachloride → (2Z)-2-(5-amino-1,2,4-thiadiazol-3-yl)-2-methoxyiminoacetyl chloride;hydrochloride

HRID 1088247

반응식

HRID 1088247 반응식
P(Cl)(Cl)(Cl)(Cl)[Cl:2].[NH2:7][C:8]1[S:12][N:11]=[C:10](/[C:13](=[N:17]/[O:18][CH3:19])/[C:14](O)=[O:15])[N:9]=1>C(Cl)Cl>[ClH:2].[NH2:7][C:8]1[S:12][N:11]=[C:10](/[C:13](=[N:17]/[O:18][CH3:19])/[C:14]([Cl:2])=[O:15])[N:9]=1

참가 물질

4

반응물 2

HCID 24819Phosphorus pentachlorideHCID 101304122-(5-Amino-1,2,4-thiadiazol-3-yl)-2-(methoxyimino)acetic acid

생성물 1

HCID 19930550(2Z)-2-(5-amino-1,2,4-thiadiazol-3-yl)-2-methoxyiminoacetyl chloride;hydrochloride

시약·촉매·용매 1

HCID 6344Dichloromethane용매

반응 조건

온도
-20 °C

실험 절차

To a solution of 218 mg of phosphorus pentachloride in 3 ml of methylene chloride, 202 mg of 2-(5-amino-1,2,4-thiadiazol-3-yl)-2(Z)-methoxyiminoacetic acid is added under cooling at -20° C. with stirring and the mixture is stirred for half an hour at -20° C. and for two hours at -5° C. The reaction mixture in concentrated under reduced pressure and the residue is triturated with 10 ml of hexane. The precipitate is collected by filtration to give 2-(5-amino-1,2,4-thiadiazol-3-yl)-2(Z)-methoxyiminoacetyl chloride hydrochloride.

후처리

  1. stirringthe mixture is stirred for half an hour at -20° C. and for two hours at -5° C
  2. concentrationThe reaction mixture in concentrated under reduced pressure
  3. customthe residue is triturated with 10 ml of hexane
  4. filtrationThe precipitate is collected by filtration

출처 및 근거

ORD 기록
ord-b725842e01dc4fee9d6796f94044609a
출처 데이터셋
uspto-grants-1990_10
특허 번호
US04962100

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