Hydrochloric Acid → Sulfametrole

HRID 26634노트

반응식

HRID 26634 반응식
[CH3:1][O:2][C:3]1[C:7](Cl)=[N:6][S:5][N:4]=1.CS(C)=O.[S:13]([NH2:23])(=[O:22])([C:15]1[CH:20]=[CH:19][C:18]([NH2:21])=[CH:17][CH:16]=1)=[O:14].C(=O)([O-])[O-].[K+].[K+].Cl>O>[CH3:1][O:2][C:3]1[C:7]([NH:23][S:13]([C:15]2[CH:16]=[CH:17][C:18]([NH2:21])=[CH:19][CH:20]=2)(=[O:14])=[O:22])=[N:6][S:5][N:4]=1

참가 물질

7

반응물 5

HCID 313Hydrochloric AcidHCID 679Dimethyl SulfoxideHCID 5333SulfanilamideHCID 11430Potassium CarbonateHCID 181772483-Chloro-4-methoxy-1,2,5-thiadiazole

생성물 1

HCID 64939Sulfametrole수율 94.7%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

150.6 g of 3-methoxy-4-chloro-1,2,5-thiadiazole (1 mole) were suspended in 156.26 g of dimethyl sulfoxide (2 mole) and 258.31 g of sulfanilamide (1.5 mole) and 414.63 g of potassium carbonate (3 mole) were then added. The mixture was kept at 70° C. for 48 hours while stirring. 600 ml of water were then added, the mixture was cooled to ambient temperature and adjusted to pH 1.5 with concentrated hydrochloric acid. The precipitated crystallized material was filtered off, washed with water and dried. A yield of 271.1 g of crude 3-methoxy-4-(4'-aminobenzenesulfonamido)-1,2,5-thiadiazole (94.67% of theory), melting point 138°-146° C., was obtained.

후처리

  1. customThe precipitated crystallized material
  2. filtrationwas filtered off
  3. washwashed with water
  4. customdried

출처 및 근거

ORD 기록
ord-465fd41c1f3c446db97935adfb6ccdaa
출처 데이터셋
uspto-grants-1979_04
특허 번호
US04151164

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