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

HRID 979075

反応式

HRID 979075 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.[K+].[K+].[Cl:27]Cl.O>C(O)(=O)C>[Cl:27][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 24502Potassium DichromateHCID 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-phenothiazin-3-one in 12.5 liters of glacial acetic acid was added 1.25 kg of potassium 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 liters of H2O with vigorous stirring. The 4-chloro-3H-phenothiazin-3-one which precipitated was allowed to settle overnight. The majority of the aqueous solution was siphoned off 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-chloro-3H-phenothiazin-3-one which was recrystallized from toluene. m.p.: 221° C.

後処理

  1. additionwas added
  2. stirringwas stirred at room temperature for another 1/2 hour
  3. customThe 4-chloro-3H-phenothiazin-3-one which 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-387104af48ff4ad7bf8e7a672d96f8f6
出典データセット
uspto-grants-1987_05
特許番号
US04666907

関連ノート

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