Trifluoroacetic anhydride → 8-Bromoisoquinolin-1-ol

HRID 1437357노트

반응식

HRID 1437357 반응식
[Br:1][C:2]1[CH:3]=[CH:4][CH:5]=[C:6]2[C:11]=1[CH:10]=[N+:9]([O-])[CH:8]=[CH:7]2.FC(F)(F)C(OC(=O)C(F)(F)F)=[O:16]>CN(C=O)C>[Br:1][C:2]1[CH:3]=[CH:4][CH:5]=[C:6]2[C:11]=1[C:10](=[O:16])[NH:9][CH:8]=[CH:7]2

참가 물질

4

반응물 2

HCID 9845Trifluoroacetic anhydrideHCID 687005028-Bromoisoquinoline 2-oxide

생성물 1

HCID 529877478-Bromoisoquinolin-1-ol

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A suspension of (a) (630 mg, 2.8 mmol) in DMF (10 ml) was treated with trifluoroacetic acid anhydride (4 ml). The clear solution was stirred at room temperature overnight then evaporated. The residue was treated with dilute aqueous sodium carbonate solution and extracted several times with 5% methanol/dichloromethane. The combined organic extracts were washed with brine, dried and evaporated. The crude product was chromatographed on silica eluting with 0-10% methanol in dichloromethane affording a white solid (180 mg, 29%).

후처리

  1. customthen evaporated
  2. additionThe residue was treated with dilute aqueous sodium carbonate solution
  3. extractionextracted several times with 5% methanol/dichloromethane
  4. washThe combined organic extracts were washed with brine
  5. customdried
  6. customevaporated
  7. customThe crude product was chromatographed on silica eluting with 0-10% methanol in dichloromethane affording a white solid (180 mg, 29%)

출처 및 근거

ORD 기록
ord-b1a18a6a42b64951901f50a23ac55719
출처 데이터셋
uspto-grants-2009_11
특허 번호
US07622481B2

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