Methyl iodide → HCID 178464747、化合物

HRID 1111057

反応式

HRID 1111057 の反応式
C(NC(N)=S)C.CI.I.C(NC(=N)SC)C.[C:17](Cl)(=[O:24])[C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1.[OH-].[Na+].[C:28]([N:36](CC)[C:37](=[N:40][C:41](=O)[C:42]1C=CC=CC=1)SC)(=[O:35])[C:29]1[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=1.C(N(C(=O)C1C=CC=CC=1)C(=N)S)(=O)C1C=CC=CC=1.Cl.[NH2:72][CH2:73][C:74]1[CH:79]=[CH:78][C:77]([S:80]([NH2:83])(=[O:82])=[O:81])=[CH:76][CH:75]=1.C([O-])(=O)C.[Na+]>C(O)(C)C.CC(C)=O>[NH2:83][S:80]([C:77]1[CH:76]=[CH:75][C:74]([CH2:73][NH:72][C:37](=[N:36][C:28](=[O:35])[C:29]2[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=2)[N:40]([CH2:41][CH3:42])[C:17](=[O:24])[C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)=[CH:79][CH:78]=1)(=[O:81])=[O:82]

参加物

12

反応物 9

HCID 6328Methyl iodideHCID 7412Benzoyl chlorideHCID 14798Sodium HydroxideHCID 67313Mafenide HydrochlorideHCID 517045Sodium AcetateHCID 3032338EthylthioureaHCID 221545061,3-Bisbenzoyl-1-ethyl-2-methylisothioureaHCID 178464634HCID 178464634、化合物HCID 178514169HCID 178514169、化合物

生成物 1

HCID 178464747HCID 178464747、化合物

試薬・触媒・溶媒 2

HCID 180Acetone溶媒HCID 3776Isopropanol溶媒

実験手順

To 36 g. of 1-ethylthiourea in 200 ml. of acetone was added 70 g. of methyliodide. Evaporation of the solvent gave 71 g. of 1-ethyl-2-methylisothiourea hydroiodide as colorless crystals, m.p. 84°-87° C. This isothiurea, 23.2 g., was reacted with a total of 30 ml. of benzoyl chloride and after 6 hours the solution was poured onto ice. The mixture was made basic with NaOH and the crystals which formed were collected by filtration to give 27.8 g. of 1,3-bisbenzoyl-1-ethyl-2-methylisothiourea, m.p. 84°-86° C. This bisbenzoylisothiourea, 3.1 g., was reacted with 2.4 g. of 4-aminomethylbenzenesulfonamide hydrochloride and 1.5 g. of sodium acetate in 250 ml. of isopropyl alcohol. Aqueous work-up followed by dichloromathane extraction and evaporation gave the title compound as a colorless glass, m.p. 70°-80° C.

後処理

  1. customEvaporation of the solvent
  2. customgave 71 g
  3. custom, was reacted with a total of 30 ml
  4. customthe crystals which formed
  5. filtrationwere collected by filtration
  6. customto give 27.8 g
  7. custom, was reacted with 2.4 g
  8. extractionAqueous work-up followed by dichloromathane extraction and evaporation

出典と根拠

ORDレコード
ord-e672424bc46e4ba99cfb0f8c6788beb2
出典データセット
uspto-grants-1990_12
特許番号
US04977189

関連ノート

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