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Phosphorus oxide (P4O10) → 3,5-Diphenyl-1H-pyrazolo[4,3-c]isoquinoline

HRID 1760164
ノート
印刷プレビュー

反応式

HRID 1760164 の反応式
O=P12OP3(OP(OP(O3)(O1)=O)(=O)O2)=O.[C:15]1([C:21]2[C:25]([NH:26][CH2:27][C:28]3[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=3)=[C:24]([C:34]3[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=3)[NH:23][N:22]=2)[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1.P(Cl)(Cl)(Cl)=O.C(=O)([O-])O.[Na+]>C1(C)C(C)=CC=CC=1>[C:15]1([C:21]2[C:25]3[N:26]=[C:27]([C:28]4[CH:29]=[CH:30][CH:31]=[CH:32][CH:33]=4)[C:39]4[CH:38]=[CH:37][CH:36]=[CH:35][C:34]=4[C:24]=3[NH:23][N:22]=2)[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 14812Phosphorus oxide (P4O10)HCID 24813Phosphorus oxychlorideHCID 516892Sodium BicarbonateHCID 12094555HCID 12094555、化合物

生成物 1

HCID 100874193,5-Diphenyl-1H-pyrazolo[4,3-c]isoquinoline

試薬・触媒・溶媒 1

HCID 7237O-Xylene溶媒

反応条件

温度
150 °C

実験手順

201 mg of phosphorus pentoxide were added to a solution of 240 mg of N-(3,5-diphenyl-1H-pyrazol-4-yl)benzylamine (2) in 10 ml of xylene, after which 195 μl of phosphorus oxychloride were added dropwise at 150° C. The reaction solution was stirred at 150° C. for 4 h and then stirred at RT for 12 h; a saturated solution of sodium hydrogen carbonate was then added and the whole was extracted with methylene chloride. The organic phase was dried over magnesium sulfate, concentrated under reduced pressure and purified by means of HPLC (Merk-Hibar-Lichrospher 100-RP-18, water (0.1% trifluoroacetic acid)/acetonitrile (0.1% trifluoroacetic acid)=80/20→10/90). The following was obtained: 1. C22H15N3 (321.38); MS (ESI) 322 (M+H)

後処理

  1. stirringstirred at RT for 12 h
  2. extractionthe whole was extracted with methylene chloride
  3. dry with materialThe organic phase was dried over magnesium sulfate
  4. concentrationconcentrated under reduced pressure
  5. custompurified by means of HPLC (Merk-Hibar-Lichrospher 100-RP-18, water (0.1% trifluoroacetic acid)/acetonitrile (0.1% trifluoroacetic acid)=80/20→10/90)
  6. customThe following was obtained

出典と根拠

ORDレコード
ord-5df9ce1b75f54d6eb26223589d1240f5
出典データセット
uspto-grants-2005_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06841556B2

反応ノート

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