Sodium Carbonate → 3-[4-(2-Acetylhydrazino)phenyl]rhodanine

HRID 1679244

反応式

HRID 1679244 の反応式
C(=O)([O-])[O-].[Na+].[Na+].C(CS[C:12](=[S:18])[S:13][CH2:14][C:15]([OH:17])=O)(O)=O.[C:19]([NH:22][NH:23][C:24]1[CH:29]=[CH:28][C:27]([NH2:30])=[CH:26][CH:25]=1)(=[O:21])[CH3:20]>O>[C:19]([NH:22][NH:23][C:24]1[CH:29]=[CH:28][C:27]([N:30]2[C:15](=[O:17])[CH2:14][S:13][C:12]2=[S:18])=[CH:26][CH:25]=1)(=[O:21])[CH3:20]

参加物

5

反応物 3

HCID 10340Sodium CarbonateHCID 806183,5-Dithia-4-thioxo-1,7-heptanedioic acidHCID 81068Acetic acid, 2-(4-aminophenyl)hydrazide

生成物 1

HCID 203621233-[4-(2-Acetylhydrazino)phenyl]rhodanine

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

Sodium carbonate (1.06g. 0.010 mole) was dissolved in water (100 ml). Bis(carboxymethyl)trithiocarbonate (4.52g, 0.02 mole) was added portionwise with vigorous stirring. When solution was complete, the reaction mixture was warmed to 80°-85° C and 1-acetyl-2-(4-aminophenyl)hydrazine (3.30 g, 0.020 moles) was added in one portion. The reaction mixture was heated with stirring for 11/2 hours, cooled to about 50°-60° C, then reheated at 80°-85° C. The product began to precipitate during reheating. After another 2 hours of heating the mixture was cooled to room temperature, chilled and filtered. The solid which was collected was washed with water and dried. Yield 2.95g (53%), mp 210°-213° C (dec).

後処理

  1. temperaturethe reaction mixture was warmed to 80°-85° C
  2. temperatureThe reaction mixture was heated
  3. temperaturecooled to about 50°-60° C
  4. customreheated at 80°-85° C
  5. customto precipitate
  6. temperatureAfter another 2 hours of heating the mixture
  7. temperaturechilled
  8. filtrationfiltered
  9. customThe solid which was collected
  10. washwas washed with water
  11. customdried

出典と根拠

ORDレコード
ord-6aac6c739c0742c7af0af338a0779eee
出典データセット
uspto-grants-1978_03
特許番号
US04080207

関連ノート

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