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

HRID 231041

반응식

HRID 231041 반응식
[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

참가 물질

6

반응물 4

HCID 962WaterHCID 24502Potassium DichromateHCID 24526Chlorine3회HCID 68485Phenothiazone

생성물 1

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

시약·촉매·용매 1

HCID 176Acetic Acid용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-e91534cb4aa241b5be5599bf213ba2e3
출처 데이터셋
uspto-grants-1989_07
특허 번호
US04845083

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