Phosphorus sulfide (P2S5) → 1-Methyl-5-Methoxy-2-Indolinethione

HRID 1086511ノート

反応式

HRID 1086511 の反応式
C(=O)(O)[O-].[Na+].[CH3:6][O:7][C:8]1[CH:9]=[C:10]2[C:14](=[CH:15][CH:16]=1)[N:13]([CH3:17])[C:12](=O)[CH2:11]2.P12(SP3(SP(SP(S3)(S1)=S)(=S)S2)=S)=[S:20]>O1CCCC1>[CH3:17][N:13]1[C:14]2[C:10](=[CH:9][C:8]([O:7][CH3:6])=[CH:16][CH:15]=2)[CH2:11][C:12]1=[S:20]

参加物

5

反応物 3

HCID 14817Phosphorus sulfide (P2S5)HCID 516892Sodium BicarbonateHCID 91021941,3-Dihydro-5-methoxy-1-methyl-2H-indol-2-one

生成物 1

HCID 137767581-Methyl-5-Methoxy-2-Indolinethione

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
50 °C

実験手順

18.5 g (0.22 mol) of sodium bicarbonate are added to a solution of 19.5 g (0.11 mol) of 5-methoxy-1-methyl-2-indolinone prepared according to A. H. BECKETT, R. W. DAISLEY and J. WALKER (Tetrahedron 1968, 24 6093) and 16.5 g (0.037 mol) of phosphorus pentasulfide in 200 ml of tetrahydrofuran. The reaction medium is heated to a temperature of 50° C. for 1 h 30 min and then filtered and concentrated on a water bath under vacuum. The residue is taken up with ice-cold water and the mixture is extracted with methylene chloride. The organic phase is washed with saturated sodium chloride solution, dried and evaporated. The residue is used in the next stage without further treatment.

後処理

  1. customprepared
  2. filtrationfiltered
  3. concentrationconcentrated on a water bath under vacuum
  4. extractionthe mixture is extracted with methylene chloride
  5. washThe organic phase is washed with saturated sodium chloride solution
  6. customdried
  7. customevaporated

出典と根拠

ORDレコード
ord-5b94579deea04c9a84ebb9428ed474c1
出典データセット
uspto-grants-1991_07
特許番号
US05030646

反応ノート

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