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

HRID 1489230노트

반응식

HRID 1489230 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-f3ba7dbcc8314bcc8cd266eaa95673ec
출처 데이터셋
uspto-grants-1997_10
특허 번호
US05677319

반응 노트

불러오는 중…