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

HRID 1649567ノート

反応式

HRID 1649567 の反応式
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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-dc95acb25ef34d34b910c7c18be3458a
出典データセット
uspto-grants-1983_11
特許番号
US04418138

反応ノート

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