2-Amino-4-methoxy-6-methyl-1,3,5-triazine → N-(3-Chloropyridazine-6-sulfonyl)-N'-(4-methoxy-6-methyl-1,3,5-triazin-2-yl)urea

HRID 247469

反応式

HRID 247469 の反応式
[Cl:1][C:2]1[N:3]=[N:4][C:5]([S:8]([N:11](C2C=CC=CC=2)[C:12](=[O:14])[O-])(=[O:10])=[O:9])=[CH:6][CH:7]=1.[NH2:21][C:22]1[N:27]=[C:26]([O:28][CH3:29])[N:25]=[C:24]([CH3:30])[N:23]=1>O1CCOCC1>[Cl:1][C:2]1[N:3]=[N:4][C:5]([S:8]([NH:11][C:12]([NH:21][C:22]2[N:27]=[C:26]([O:28][CH3:29])[N:25]=[C:24]([CH3:30])[N:23]=2)=[O:14])(=[O:9])=[O:10])=[CH:6][CH:7]=1

参加物

4

反応物 2

HCID 154662-Amino-4-methoxy-6-methyl-1,3,5-triazineHCID 86741701N-(3-chloropyridazine-6-sulfonyl)phenylcarbamate

生成物 1

HCID 21275743N-(3-Chloropyridazine-6-sulfonyl)-N'-(4-methoxy-6-methyl-1,3,5-triazin-2-yl)urea収率 43.3%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

A mixture of 14.2 g of N-(3-chloropyridazine-6-sulfonyl)phenylcarbamate and 6.3 g of 2-amino-4-methoxy-6-methyl-1,3,5-triazine are refluxed for 1 hour in 120 ml of absolute dioxan. When the reaction is complete, the mixture is concentrated in vacuo and the residue is taken up in a saturated aqueous solution of sodium bicarbonate and the insoluble constituents are extracted with methylene chloride. The aqueous phase is acidified with dilute hydrochloric acid and extracted with methylene chloride. The methylene chloride solution is dried over sodium sulfate and concentrated, affording 7 g of the compound of the above formula with a melting point of 135° C.

後処理

  1. concentrationthe mixture is concentrated in vacuo
  2. extractionthe insoluble constituents are extracted with methylene chloride
  3. extractionextracted with methylene chloride
  4. dry with materialThe methylene chloride solution is dried over sodium sulfate
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-cc3cf87295054356b17909d3b9a248d0
出典データセット
uspto-grants-1987_11
特許番号
US04707551

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