Azobisisobutyronitrile → 6-(Bromomethyl)-5-(4-nitrophenyl)thieno[2,3-d]pyrimidin-4-amine

HRID 227606노트

반응식

HRID 227606 반응식
[CH3:1][C:2]1[S:11][C:5]2[N:6]=[CH:7][N:8]=[C:9]([NH2:10])[C:4]=2[C:3]=1[C:12]1[CH:17]=[CH:16][C:15]([N+:18]([O-:20])=[O:19])=[CH:14][CH:13]=1.C1C(=O)N([Br:28])C(=O)C1.CC(N=NC(C#N)(C)C)(C#N)C>C1C=CC=CC=1>[Br:28][CH2:1][C:2]1[S:11][C:5]2[N:6]=[CH:7][N:8]=[C:9]([NH2:10])[C:4]=2[C:3]=1[C:12]1[CH:13]=[CH:14][C:15]([N+:18]([O-:20])=[O:19])=[CH:16][CH:17]=1

참가 물질

5

반응물 3

HCID 6547AzobisisobutyronitrileHCID 67184N-bromobutanimideHCID 116162046-Methyl-5-(4-nitrophenyl)thieno[2,3-d]pyrimidin-4-amine

생성물 1

HCID 590995626-(Bromomethyl)-5-(4-nitrophenyl)thieno[2,3-d]pyrimidin-4-amine

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

A suspension of Example 1D (500 mg, 1.75 mmol) in benzene (50 mL) was treated with NBS (340 mg, 1.91 mmol) and AIBN (50 mg), stirred at reflux for 3.5 hours, and concentrated. The concentrate was absorbed onto silica gel and purified by flash column chromatography with ethyl acetate to provide 330 mg of a 1.7:1 mixture of the desired product and recovered starting material.

후처리

  1. temperatureat reflux for 3.5 hours
  2. concentrationconcentrated
  3. customThe concentrate was absorbed onto silica gel
  4. custompurified by flash column chromatography with ethyl acetate
  5. customto provide

출처 및 근거

ORD 기록
ord-c83ecd474b394e848d25bff6ff61dd27
출처 데이터셋
uspto-grants-2009_07
특허 번호
US07560552B2

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