Hydrochloric Acid → Sulfametrole

HRID 26634ノート

反応式

HRID 26634 の反応式
[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

参加物

7

反応物 5

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

生成物 1

HCID 64939Sulfametrole収率 94.7%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-465fd41c1f3c446db97935adfb6ccdaa
出典データセット
uspto-grants-1979_04
特許番号
US04151164

反応ノート

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