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Phenyl Isothiocyanate → HCID 178462481、化合物

HRID 1925171
ノート
印刷プレビュー

反応式

HRID 1925171 の反応式
[NH:1]([C:3]1[N:8]=[CH:7][C:6]([C:9]2[CH:10]=[CH:11][C:12](=[O:17])[N:13]([CH2:15][CH3:16])[CH:14]=2)=[CH:5][CH:4]=1)[NH2:2].N(C1C=CC=CC=1)=[C:19]=[S:20]>CN1C(=O)CCC1.C(Cl)Cl>[SH:20][C:19]1[N:8]2[CH:7]=[C:6]([C:9]3[CH:10]=[CH:11][C:12](=[O:17])[N:13]([CH2:15][CH3:16])[CH:14]=3)[CH:5]=[CH:4][C:3]2=[N:1][N:2]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 7673Phenyl IsothiocyanateHCID 592332085-(6-hydrazinylpyridin-3-yl)-1-ethylpyridin-2(1H)-one

生成物 1

HCID 178462481HCID 178462481、化合物収率 42.3%

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 13387N-methyl-2-pyrrolidone溶媒

実験手順

A mixture of 5-(6-hydrazinylpyridin-3-yl)-1-ethylpyridin-2(1 H)-one (1.2 g, 5.22 mmol) and isothiocyanatobenzene (775 mg, 5.74 mmol) in NMP(3 ml) and DCM (10 ml) was stirred at room temperature for 30 min. The DCM was removed via rotary evaporation and the reaction was diluted with 1,3-dichlorobenzene (7 mL). The mixture was then heated in a microwave at 160° C. for 1 hr. Ether (10 ml) was added to the reaction and the resulting solid was collected by filtration and washed with ether to provide the title compound, 5-(3-mercapto-[1,2,4]triazolo[4,3-a]pyridin-6-yl)-1-ethylpyridin-2(1 H)-one (600 mg, 42.3% yield).

後処理

  1. customThe DCM was removed via rotary evaporation
  2. additionthe reaction was diluted with 1,3-dichlorobenzene (7 mL)
  3. temperatureThe mixture was then heated in a microwave at 160° C. for 1 hr
  4. additionEther (10 ml) was added to the reaction
  5. filtrationthe resulting solid was collected by filtration
  6. washwashed with ether

出典と根拠

ORDレコード
ord-15f5a1c3e74d429196390a6d336649cd
出典データセット
uspto-grants-2012_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08178534B2

反応ノート

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