Methanol → 2-Chloro-8-fluoroindolo[2,1-b]quinazoline-6,12-dione

HRID 1756563

반응식

HRID 1756563 반응식
[H-].[Na+].[F:3][C:4]1[CH:5]=[C:6]2[C:10](=[CH:11][CH:12]=1)[NH:9][C:8](=O)[C:7]2=[O:14].[Cl:15][C:16]1[CH:27]=[C:20]2[C:21](OC(=O)[NH:25][C:19]2=[CH:18][CH:17]=1)=[O:22].CO>CN(C=O)C.C(Cl)(Cl)Cl>[Cl:15][C:16]1[CH:27]=[C:20]2[C:19](=[CH:18][CH:17]=1)[N:25]=[C:8]1[C:7](=[O:14])[C:6]3[C:10]([N:9]1[C:21]2=[O:22])=[CH:11][CH:12]=[C:4]([F:3])[CH:5]=3

참가 물질

7

반응물 4

HCID 887MethanolHCID 24758Sodium hydrideHCID 784805-Chloroisatoic anhydrideHCID 2365665-Fluoroisatin

생성물 1

HCID 4785692-Chloro-8-fluoroindolo[2,1-b]quinazoline-6,12-dione

시약·촉매·용매 2

HCID 6212Chloroform용매HCID 6228Dimethylformamide용매3회

실험 절차

To a suspension of NaH (10 mmol, 40 mg 60%) in 4 mL of DMF was added 10 mmol of 5-fluoroisatin in 2 mL of DMF. After 15 min, a solution of 5-chloroisatoic anhydride in 3 mL of DMF was added. The reaction mixture was stirred for 18 h, methanol (0.5 mL) and 20 mL of chloroform was added and the organic solution was washed with water, dried (MgSO4) and concentrated to give a residue which was purified by silica gel chromatography (CHCl3 :CH3OH). Yield 77%: mp 280°-282° C.

후처리

  1. washthe organic solution was washed with water
  2. dry with materialdried (MgSO4)
  3. concentrationconcentrated
  4. customto give a residue which
  5. customwas purified by silica gel chromatography (CHCl3 :CH3OH)

출처 및 근거

ORD 기록
ord-0cfebdd3820a4315bfe8dcf209410365
출처 데이터셋
uspto-grants-1995_08
특허 번호
US05441955

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