Iodine → HCID 87073288, 화합물

HRID 76134노트

반응식

HRID 76134 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

HCID 87073288HCID 87073288, 화합물

시약·촉매·용매 1

HCID 5943Carbon Tetrachloride용매

반응 조건

온도
0 °C

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-21d75c1bda0b448790fc29346dcf135d
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08835472B2

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