Phosphorus sulfide (P2S5) → Benzamide, thio-3,4,5-trimethoxy-

HRID 1489230ノート

反応式

HRID 1489230 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:9]=[C:10]([O:14][CH3:15])[C:11]=1[O:12][CH3:13])[C:6]([NH2:8])=O.P12(SP3(SP(SP(S3)(S1)=S)(=S)S2)=S)=[S:17]>C1C=CC=CC=1>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:9]=[C:10]([O:14][CH3:15])[C:11]=1[O:12][CH3:13])[C:6]([NH2:8])=[S:17]

参加物

4

反応物 2

HCID 14817Phosphorus sulfide (P2S5)HCID 183343,4,5-Trimethoxybenzamide

生成物 1

HCID 3033195Benzamide, thio-3,4,5-trimethoxy-収率 122.7%

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

500 mg of 3,4,5-trimethoxybenzamide was suspended in 15 ml of benzene. Thereto was added 526 mg of phosphorus pentasulfide. The mixture was refluxed for 30 minutes with heating. The solvent was removed by distillation. To the residue were added 5 ml of 10% sodium hydroxide and 5 ml of water. The mixture was stirred for 30 minutes. The reaction mixture was filtered, and the resulting solid was washed with small amounts of water and ethanol and dried to obtain 330 mg of 3,4,5-trimethoxythiobenzamide as a yellow powder.

後処理

  1. temperatureThe mixture was refluxed for 30 minutes
  2. temperaturewith heating
  3. customThe solvent was removed by distillation
  4. additionTo the residue were added 5 ml of 10% sodium hydroxide and 5 ml of water
  5. filtrationThe reaction mixture was filtered
  6. washthe resulting solid was washed with small amounts of water and ethanol
  7. customdried

出典と根拠

ORDレコード
ord-f3ba7dbcc8314bcc8cd266eaa95673ec
出典データセット
uspto-grants-1997_10
特許番号
US05677319

反応ノート

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