Ethylorthoformate → 6,7-dichloro-4-cyclopropyl-4H-1,2,4-benzothiadiazine 1,1-dioxide

HRID 17836

反応式

HRID 17836 の反応式
[Cl:1][C:2]1[C:7]([Cl:8])=[CH:6][C:5]([S:9]([NH2:12])(=[O:11])=[O:10])=[C:4]([NH:13][CH:14]2[CH2:16][CH2:15]2)[CH:3]=1.[CH:17]([O-])([O-])OCC>>[Cl:1][C:2]1[C:7]([Cl:8])=[CH:6][C:5]2[S:9](=[O:10])(=[O:11])[N:12]=[CH:17][N:13]([CH:14]3[CH2:16][CH2:15]3)[C:4]=2[CH:3]=1

参加物

3

反応物 2

HCID 53630039EthylorthoformateHCID 675298334,5-Dichloro-2-cyclopropylaminobenzenesulphonamide

生成物 1

HCID 675306506,7-dichloro-4-cyclopropyl-4H-1,2,4-benzothiadiazine 1,1-dioxide

反応条件

温度
150 °C

実験手順

In a round-bottom flask, a mixture of 4,5-dichloro-2-cyclopropylaminobenzenesulphonamide from the Step above (2.5 g) and ethyl orthoformate (25 mL) is heated in the open state at 150° C. for 1 hour. The suspension obtained is cooled on an ice bath, and the insoluble material is collected by filtration, washed with ether and dried. The solid is re-dissolved in a mixture of acetone and methanol in the hot state and the hot solution is treated with absorbent carbon and then filtered and concentrated to dryness. The residue is recrystallised from methanol.

後処理

  1. customThe suspension obtained
  2. temperatureis cooled on an ice bath
  3. filtrationthe insoluble material is collected by filtration
  4. washwashed with ether
  5. customdried
  6. dissolutionThe solid is re-dissolved in a mixture of acetone and methanol in the hot state
  7. additionthe hot solution is treated with absorbent carbon
  8. filtrationfiltered
  9. concentrationconcentrated to dryness
  10. customThe residue is recrystallised from methanol

出典と根拠

ORDレコード
ord-7b7f45fc90a3465183bb7ac4ccf35df4
出典データセット
uspto-grants-2010_06
特許番号
US07741320B2

関連ノート

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