4-Bromo-7-nitrobenzo[c][1,2,5]oxadiazole → HCID 21875029, 화합물

HRID 1441808노트

반응식

HRID 1441808 반응식
[Br:1][C:2]1[C:7]2=[N:8][O:9][N:10]=[C:6]2[C:5]([N+:11]([O-])=O)=[CH:4][CH:3]=1>CC(O)=O>[Br:1][C:2]1[C:7]2=[N:8][O:9][N:10]=[C:6]2[C:5]([NH2:11])=[CH:4][CH:3]=1

참가 물질

3

반응물 1

HCID 120102144-Bromo-7-nitrobenzo[c][1,2,5]oxadiazole

생성물 1

HCID 21875029HCID 21875029, 화합물수율 95.1%

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

A solution of compound 422A (563 mg, 2.31 mmol) in AcOH (5 mL) was heated to 70° C. and Fe0 powder (258 mg, 4.62 mmol) was added in one portion. The resulting dark reaction mixture was stirred for 15 min, cooled to rt and concentrated under reduced pressure. The residue was taken up in EtOAc and the resulting solution was washed with sat. Na2CO3 solution. The organic layer was dried over Na2SO4, concentrated in vacuo and purified by flash chromatography on silica gel eluting with 10-60% EtOAc in hexanes to give 470 mg (95%) of compound 422B as a red solid.

후처리

  1. customThe resulting dark reaction mixture
  2. concentrationconcentrated under reduced pressure
  3. washthe resulting solution was washed with sat. Na2CO3 solution
  4. dry with materialThe organic layer was dried over Na2SO4
  5. concentrationconcentrated in vacuo
  6. custompurified by flash chromatography on silica gel eluting with 10-60% EtOAc in hexanes

출처 및 근거

ORD 기록
ord-112470a5cb544fdbbcb9bfb5742ce261
출처 데이터셋
uspto-grants-2010_02
특허 번호
US07655689B2

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