Sulfuric Acid → 2-Hydroxy-3,4-dimethyl-9H-thioxanthen-9-one

HRID 1462230노트

반응식

HRID 1462230 반응식
S(=O)(=O)(O)O.[C:6]([OH:15])(=O)[C:7]1[C:8](=[CH:10][CH:11]=[CH:12][CH:13]=1)[SH:9].[CH3:16][C:17]1[C:22]([CH3:23])=[CH:21][CH:20]=[CH:19][C:18]=1[OH:24]>O>[OH:24][C:18]1[C:17]([CH3:16])=[C:22]([CH3:23])[C:21]2[S:9][C:8]3[C:7](=[CH:13][CH:12]=[CH:11][CH:10]=3)[C:6](=[O:15])[C:20]=2[CH:19]=1

참가 물질

5

반응물 3

HCID 1118Sulfuric AcidHCID 54432-Mercaptobenzoic AcidHCID 106872,3-Dimethylphenol

생성물 1

HCID 135937022-Hydroxy-3,4-dimethyl-9H-thioxanthen-9-one

시약·촉매·용매 1

HCID 962Water용매

실험 절차

Concentrated sulphuric acid (300 ml) was slowly added to thiosalicylic acid (30.9 g) and the mixture was stirred for 5 minutes to ensure thorough mixing. To the stirred mixture was added slowly over a period of 30 minutes 2,3-dimethyl-phenol (138 g). After the addition, the mixture was stirred at room temperature for 1 hour, and then at 80° C. for 2 hours, after which it was left to stand at room temperature overnight. The resulting mixture was poured carefully with stirring into 10 times its volume of boiling water after which it was boiled for a further five minutes, cooled, and filtered. The residue was recrystallised from acetone to give 2-hydroxy-3,4-dimethyl-thioxanthone as a yellow product.

후처리

  1. additionAfter the addition
  2. stirringthe mixture was stirred at room temperature for 1 hour
  3. waitat 80° C. for 2 hours
  4. waitafter which it was left
  5. waitto stand at room temperature overnight
  6. additionThe resulting mixture was poured carefully
  7. waitwas boiled for a further five minutes
  8. temperaturecooled
  9. filtrationfiltered
  10. customThe residue was recrystallised from acetone

출처 및 근거

ORD 기록
ord-44859123e4114ca8971d628ceed3f15a
출처 데이터셋
uspto-grants-1984_07
특허 번호
US04459416

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