Water → 3H-Phenothiazin-3-one, 4-chloro-

HRID 2352231

反応式

HRID 2352231 の反応式
[CH:1]1[C:14]2[C:5]([S:6][C:7]3[C:12]([N:13]=2)=[CH:11][CH:10]=[CH:9][CH:8]=3)=[CH:4][C:3](=[O:15])[CH:2]=1.[Cr](O[Cr]([O-])(=O)=O)([O-])(=O)=O.[Cl:25]Cl.O>C(O)(=O)C>[Cl:25][C:4]1[C:3](=[O:15])[CH:2]=[CH:1][C:14]2[C:5]=1[S:6][C:7]1[C:12](=[CH:11][CH:10]=[CH:9][CH:8]=1)[N:13]=2

参加物

6

反応物 4

HCID 962WaterHCID 24503Dichromate ionHCID 24526Chlorine3 回HCID 68485Phenothiazone

生成物 1

HCID 117767483H-Phenothiazin-3-one, 4-chloro-

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒2 回

実験手順

To a stirring solution of 500 g (2.34 mol) of 3H-phenothiaz-3-one in 12.5 L of glacia acetic acid was added 1.25 kg of ptassium dichromate. The mixture was stirred at room temperature for 1/2 hour. To this resulting mixture was then added 2.34 mol of a 1M solution of chlorine in glacial acetic acid dropwise over a period of 4 hours. The progress of the reaction was monitored by tlc to ensure no excess chlorine was added. After addition of chlorine was completed the mixture was stirred at room temperature for another 1/2 hour and was then poured into 120 L of H2O with vigorous stirring. The 4-chlorophenothiazin-3-one precipitated was allowed to settle overnight. The majority of the aqueous solution was siphoned and discarded and the rest was filtered. The filtered precipitate was washed thoroughly with water and then rinsed with methanol and was allowed to dry to give 504 g crude 4-chlorophenothiazin-3-one which was recrystallized from toluene.

後処理

  1. additionwas added
  2. stirringwas stirred at room temperature for another 1/2 hour
  3. customThe 4-chlorophenothiazin-3-one precipitated
  4. waitto settle overnight
  5. filtrationthe rest was filtered
  6. washThe filtered precipitate was washed thoroughly with water
  7. washrinsed with methanol
  8. customto dry

出典と根拠

ORDレコード
ord-a74e335f3f694d1890c0af835c50db8c
出典データセット
uspto-grants-1989_10
特許番号
US04876246

関連ノート

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