Phosphorus sulfide (P2S5) → 2,6-Diphenylthiopyrylium perchlorate

HRID 391496

反応式

HRID 391496 の反応式
[C:1]1([C:7](=O)[CH2:8][CH2:9][CH2:10][C:11]([C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)=O)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.P12(SP3(SP(SP(S3)(S1)=S)(=S)S2)=S)=[S:21].[Cl:34]([O-:38])(=[O:37])(=[O:36])=[O:35].[Li+]>C(O)(=O)C>[Cl:34]([O-:38])(=[O:37])(=[O:36])=[O:35].[C:1]1([C:7]2[CH:8]=[CH:9][CH:10]=[C:11]([C:13]3[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=3)[S+:21]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

参加物

5

反応物 3

HCID 14817Phosphorus sulfide (P2S5)HCID 804321,3-DibenzoylpropaneHCID 23665649Lithium perchlorate

生成物 1

HCID 856151432,6-Diphenylthiopyrylium perchlorate収率 24%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

The 1,5-diphenyl-1,5-pentanedione prepared in step 1 (10 mmol, 2.52 g) is mixed with phosphorus pentasulfide (15 mmol, 3.34 g), acetic acid (60 mL) and lithium perchlorate (60 mmol, 6.40 g) in a 100 mL two-necked round-bottomed flask, and then refluxed for 3 hours. The solution then becomes orange and a white precipitate forms. The precipitate is removed by filtration on a sinter funnel and then washed with hot acetic acid. The solution is concentrated on a rotary evaporator and recrystallized by addition of ether (500 mL). The precipitate obtained is filtered off on a sinter funnel and then dried on a rotary evaporator. The product obtained is a yellow solid in a mass of 850 mg. The reaction yield is 24%.

後処理

  1. temperaturerefluxed for 3 hours
  2. customThe precipitate is removed by filtration on a sinter funnel
  3. washwashed with hot acetic acid
  4. concentrationThe solution is concentrated on a rotary evaporator
  5. customrecrystallized by addition of ether (500 mL)
  6. customThe precipitate obtained
  7. filtrationis filtered off on a sinter funnel
  8. customdried on a rotary evaporator
  9. customThe product obtained
  10. customThe reaction yield is 24%

出典と根拠

ORDレコード
ord-acea0814511143e5916fdb418c642130
出典データセット
uspto-grants-2013_02
特許番号
US08383931B2

関連ノート

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