Hydrochloric Acid → HCID 178457590、化合物

HRID 1973118ノート

反応式

HRID 1973118 の反応式
[CH3:1][N:2]([CH3:13])[S:3]([C:6]1[CH:12]=[CH:11][C:9]([NH2:10])=[CH:8][CH:7]=1)(=[O:5])=[O:4].Cl.[CH:15]([NH:18][C:19]([NH:21][C:22]#[N:23])=[NH:20])([CH3:17])[CH3:16]>C(O)(C)C>[CH3:1][N:2]([CH3:13])[S:3]([C:6]1[CH:12]=[CH:11][C:9]([NH:10][C:22]([NH:21][C:19]([NH:18][CH:15]([CH3:17])[CH3:16])=[NH:20])=[NH:23])=[CH:8][CH:7]=1)(=[O:4])=[O:5]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 74369Benzenesulfonamide, 4-amino-N,N-dimethyl-HCID 178457589HCID 178457589、化合物

生成物 1

HCID 178457590HCID 178457590、化合物

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

実験手順

To 11 g (0.055 mole) of p-N,N-dimethylsulfamylaniline is added 17.68 ml (0.055) of 3.1 N hydrochloric acid. This is heated on a steam bath with 15 ml of isopropanol and 6.94 g (0.055 mole) of 1-i-propyl-3-cyanoguanidine. The reaction mixture is heated for 18 hours. The alcohol is evaporated off and diluted with 250 ml of 7.4% hydrochloric acid. The mixture is filtered, cooled and made alkaline with 10% sodium hydroxide. The precipitate is filtered, triturated with 100 ml of boiling isopropanol and filtered to get 1-(p-N,N-dimethylsulfamylphenyl)-5-i-propylbiguanide.

後処理

  1. temperatureThe reaction mixture is heated for 18 hours
  2. customThe alcohol is evaporated off
  3. additiondiluted with 250 ml of 7.4% hydrochloric acid
  4. filtrationThe mixture is filtered
  5. temperaturecooled
  6. filtrationThe precipitate is filtered
  7. customtriturated with 100 ml of boiling isopropanol
  8. filtrationfiltered

出典と根拠

ORDレコード
ord-b1318bbb444c46d1bcf266b52368b105
出典データセット
uspto-grants-1976_12
特許番号
US03996232

反応ノート

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