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Phosphorus sulfide (P2S5) → HCID 20361194, 화합물

HRID 1679577
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HRID 1679577 반응식
[CH3:1][S:2][C:3]1[CH:4]=[CH:5][C:6]2[NH:12][C:11](=O)[CH2:10][N:9]=[C:8]([C:14]3[CH:19]=[CH:18][CH:17]=[CH:16][N:15]=3)[C:7]=2[CH:20]=1.P12(SP3(SP(SP(S3)(S1)=S)(=S)S2)=S)=[S:22]>N1C=CC=CC=1>[CH3:1][S:2][C:3]1[CH:4]=[CH:5][C:6]2[NH:12][C:11](=[S:22])[CH2:10][N:9]=[C:8]([C:14]3[CH:19]=[CH:18][CH:17]=[CH:16][N:15]=3)[C:7]=2[CH:20]=1
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참가 물질

4

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HCID 14817Phosphorus sulfide (P2S5)HCID 203612567-(Methylsulfanyl)-5-(pyridin-2-yl)-1,3-dihydro-2H-1,4-benzodiazepin-2-one

생성물 1

HCID 20361194HCID 20361194, 화합물

시약·촉매·용매 1

HCID 1049Pyridine용매

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온도
115 °C

실험 절차

A stirred solution of 7-methylthio-1,3-dihydro-5-(2-pyridyl)-2H-1,4-benzodiazepin-2-one (0.0206 mole) in dry pyridine (400 ml.) was treated with phosphorus pentasulfide (5.05 g.), warmed, under nitrogen, at 110-120° C. for 1 hour, cooled and concentrated in vacuo. Residual pyridine was removed by the successive addition of xylene and toluene to the residue with concentration after each addition. The resulting residue was mixed with dilute sodium carbonate and extracted with chloroform. The chloroform extract was washed with brine, dried over anhydrous sodium sulfate and concentrated. The residue was crystallized to give 7-methylthio-1,3-dihydro-5-(2-pyridyl)-2H-1,4-benzodiazepine-2-thione.

후처리

  1. temperaturecooled
  2. concentrationconcentrated in vacuo
  3. customResidual pyridine was removed by the successive addition of xylene and toluene to the residue with concentration
  4. additionafter each addition
  5. additionThe resulting residue was mixed with dilute sodium carbonate
  6. extractionextracted with chloroform
  7. extractionThe chloroform extract
  8. washwas washed with brine
  9. dry with materialdried over anhydrous sodium sulfate
  10. concentrationconcentrated
  11. customThe residue was crystallized

출처 및 근거

ORD 기록
ord-174d39762db24f7cb8b7cbbcebc7a318
출처 데이터셋
uspto-grants-1978_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04081452

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