Lawesson's reagent → HCID 53772023、化合物

HRID 1459654ノート

反応式

HRID 1459654 の反応式
[NH2:1][C:2]([CH2:4][C:5]1[N:9]([CH2:10][C:11]2[CH:18]=[CH:17][C:14]([C:15]#[N:16])=[CH:13][CH:12]=2)[CH:8]=[N:7][CH:6]=1)=O.COC1C=CC(P2(SP(C3C=CC(OC)=CC=3)(=S)S2)=[S:28])=CC=1>O1CCOCC1>[C:15]([C:14]1[CH:17]=[CH:18][C:11]([CH2:10][N:9]2[C:5]([CH2:4][C:2]([NH2:1])=[S:28])=[CH:6][N:7]=[CH:8]2)=[CH:12][CH:13]=1)#[N:16]

参加物

4

反応物 2

HCID 87949Lawesson's reagentHCID 18393829HCID 18393829、化合物

生成物 1

HCID 53772023HCID 53772023、化合物

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

反応条件

温度
80 °C

実験手順

To a 50 mL round bottomed flask with a stirring bar, reflux condenser and an argon inlet was added 4-[5-(aminocarbonylmethyl) imidazol-1-ylmethyl]benzonitrile (0.36 g, 1.49 mmol), Lawesson's reagent (0.73 g, 1.8 mmol) and 1,4-dioxane (10 mL). This well stirred mixture was heated at 80° C. for 24 hours. The cooled reaction mixture was concentrated in vacuo and the residue was chromatographed (silica gel, 10% 2-propanol in ammonia saturated CHCl3). The title compound was obtained as a yellow, crystalline solid.

後処理

  1. temperatureTo a 50 mL round bottomed flask with a stirring bar, reflux condenser and an argon inlet
  2. customThe cooled reaction mixture
  3. concentrationwas concentrated in vacuo
  4. customthe residue was chromatographed (silica gel, 10% 2-propanol in ammonia saturated CHCl3)

出典と根拠

ORDレコード
ord-d8944a3f22ad40d782e56698223025e8
出典データセット
uspto-grants-1998_12
特許番号
US05854265

反応ノート

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