Phosphorus sulfide (P2S5) → HCID 9922428、化合物

HRID 2120752ノート

反応式

HRID 2120752 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([C:8]2[CH:9]=[C:10]3[C:15](=[CH:16][CH:17]=2)[NH:14][C:13](=O)[CH2:12][C:11]3([CH3:20])[CH3:19])[CH:5]=[CH:6][CH:7]=1.P12(SP3(SP(SP(S3)(S1)=S)(=S)S2)=S)=[S:22]>N1C=CC=CC=1>[Cl:1][C:2]1[CH:3]=[C:4]([C:8]2[CH:9]=[C:10]3[C:15](=[CH:16][CH:17]=2)[NH:14][C:13](=[S:22])[CH2:12][C:11]3([CH3:20])[CH3:19])[CH:5]=[CH:6][CH:7]=1

参加物

4

反応物 2

HCID 14817Phosphorus sulfide (P2S5)HCID 99656566-(3-chlorophenyl)-4,4-dimethyl-3,4-dihydroquinoline-2(1H)-one

生成物 1

HCID 9922428HCID 9922428、化合物

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

Prepared by heating under reflux overnight a mixture of 6-(3-chlorophenyl)-4,4-dimethyl-3,4-dihydroquinoline-2(1H)-one and an equal weight of phosphorus pentasulfide in pyridine was stirred. Removal of the pyridine in vacuo followed by treating the residue with 6N hydrochloric acid and recrystallization of the residue in ethanol gave the product as a yellow solid: mp. 197-1980 C. 1H-NMR (DMSO-d6) 8 12.34 (s, 1H), 7.75 (m, 1H), 7.64 (m, 2H), 7.57 (dd, 1H J=9.3 and 2.1 Hz), 7.48 (t, 1H, J=7.7 Hz), 7.41 (m, 1H),7.20 (d, 1H, J=8.3 Hz), 3.34 (s, 2H), 1.26 (s, 6H); MS (APCI (−)) m/z 300 [M−H]− Anal. Calc. For C17H16CINS: C, 67.65, H, 5.34, N, 4.64. Found: C, 67.77, H, 5.57, N 4.54.

後処理

  1. customPrepared
  2. temperatureby heating
  3. temperatureunder reflux overnight
  4. customRemoval of the pyridine in vacuo
  5. additionby treating the residue
  6. customwith 6N hydrochloric acid and recrystallization of the residue in ethanol

出典と根拠

ORDレコード
ord-bde40e033dea48c68ce69dae82ee8775
出典データセット
uspto-grants-2004_02
特許番号
US06693103B2

反応ノート

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