Iodine → HCID 87073288、化合物

HRID 76134ノート

反応式

HRID 76134 の反応式
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]2[N:10]=[CH:11][C:12](N)=[N:13][CH:14]=2)=[CH:5][CH:4]=1.N(OC(C)(C)C)=O.[I:23]I>C(Cl)(Cl)(Cl)Cl>[I:23][C:12]1[CH:11]=[N:10][C:9]([C:6]2[CH:7]=[CH:8][C:3]([O:2][CH3:1])=[CH:4][CH:5]=2)=[CH:14][N:13]=1

参加物

5

反応物 3

HCID 807IodineHCID 10906Tert-Butyl nitriteHCID 156743865-(4-Methoxyphenyl)pyrazin-2-amine

生成物 1

HCID 87073288HCID 87073288、化合物

試薬・触媒・溶媒 1

HCID 5943Carbon Tetrachloride溶媒

反応条件

温度
0 °C

実験手順

In a light protected flask, 4.10 g (20.4 mmol) 5-(4-methoxyphenyl)-pyrazin-2-amine are added to 140 mL carbon tetrachloride. After cooling down to 0° C. 4.12 mL (34.6 mmol) tert-butyl nitrite and 6.72 g (26.5 mmol) iodine are added sequently. Then cooling is removed and the reaction mixture is stirred at ambient temperature over night. The reaction mixture is diluted with DCM and washed sequently with aq. Na2S2O5 solution and water. The organic layer is dried with MgSO4 and the solvent is removed in vacuo. The residue is triturated with TBME and purified by column chromatography (silica gel, PE/EtOAc 6/4).

後処理

  1. temperatureThen cooling
  2. customis removed
  3. additionThe reaction mixture is diluted with DCM
  4. washwashed sequently with aq. Na2S2O5 solution and water
  5. dry with materialThe organic layer is dried with MgSO4
  6. customthe solvent is removed in vacuo
  7. customThe residue is triturated with TBME
  8. custompurified by column chromatography (silica gel, PE/EtOAc 6/4)

出典と根拠

ORDレコード
ord-21d75c1bda0b448790fc29346dcf135d
出典データセット
uspto-grants-2014_09
特許番号
US08835472B2

反応ノート

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