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Iodine → 8-Fluoro-2,2,4,11-tetramethyl-1,2-dihydro-6-oxa-1-azachrysen-5-one

HRID 909305
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인쇄 미리보기

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HRID 909305 반응식
[NH2:1][C:2]1[CH:3]=[C:4]([CH3:18])[C:5]2[C:14]3[C:9](=[CH:10][C:11]([F:15])=[CH:12][CH:13]=3)[O:8][C:7](=[O:16])[C:6]=2[CH:17]=1.II>CC(C)=O>[F:15][C:11]1[CH:10]=[C:9]2[C:14](=[CH:13][CH:12]=1)[C:5]1[C:6](=[C:17]3[C:2](=[CH:3][C:4]=1[CH3:18])[NH:1][C:4]([CH3:18])([CH3:5])[CH:3]=[C:2]3[CH3:17])[C:7](=[O:16])[O:8]2
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참가 물질

4

반응물 2

HCID 807IodineHCID 580271338-Amino-3-fluoro-10-methylbenzo[c]chromen-6-one

생성물 1

HCID 580267238-Fluoro-2,2,4,11-tetramethyl-1,2-dihydro-6-oxa-1-azachrysen-5-one수율 78%

시약·촉매·용매 1

HCID 180Acetone용매

반응 조건

온도
110 °C

실험 절차

In a pressure tube, 8-amino-3-fluoro-10-methylbenzo[c]chromen-6-one (Reference Compound No. 1-4-(6), 6.13 g, 25.2 mmol) was dissolved in acetone (175 mL) and iodine (2.56 g, 10.1 mmol) was added thereto, then the pressure tube was sealed, and then the reaction mixture was stirred at 110° C. for 4 days. After cooling down, the solvent was removed under reduced pressure. The obtained residue was purified by silica gel column chromatography (hexane-ethyl acetate) to give the titled reference compound (6.35 g) as a brown solid. (Yield 78%)

후처리

  1. customthe pressure tube was sealed
  2. temperatureAfter cooling down
  3. customthe solvent was removed under reduced pressure
  4. customThe obtained residue was purified by silica gel column chromatography (hexane-ethyl acetate)

출처 및 근거

ORD 기록
ord-f55452b3bf074f7e8c82f6d125db3d81
출처 데이터셋
uspto-grants-2011_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08017775B2

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