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Iodine → 2,2,4-Trimethyl-1,2-dihydro-6-oxa-1-azachrysen-5-one

HRID 1966259
노트
인쇄 미리보기

반응식

HRID 1966259 반응식
[NH2:1][C:2]1[CH:3]=[CH:4][C:5]2[C:14]3[C:9](=[CH:10][CH:11]=[CH:12][CH:13]=3)[O:8][C:7](=[O:15])[C:6]=2[CH:16]=1.II>CC(C)=O>[CH3:6][C:5]1([CH3:14])[CH:4]=[C:3]([CH3:2])[C:16]2[C:2](=[CH:3][CH:4]=[C:5]3[C:6]=2[C:7](=[O:15])[O:8][C:9]2[C:14]3=[CH:13][CH:12]=[CH:11][CH:10]=2)[NH:1]1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 807IodineHCID 233789368-Aminobenzo[c]chromen-6-one

생성물 1

HCID 104937872,2,4-Trimethyl-1,2-dihydro-6-oxa-1-azachrysen-5-one수율 40%

시약·촉매·용매 1

HCID 180Acetone용매

반응 조건

온도
105 °C

실험 절차

In a pressure tube, 8-aminobenzo[c]chromen-6-one (Reference Compound No. 1-1-(2), 8.81 g, 41.7 mmol) was dissolved in acetone (300 ml . . . ), then iodine (4.24 g, 16.7 mmol) was added thereto, then the pressure tube was sealed, and then the reaction mixture was stirred at 105° C. for 2 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 (4.83 g) as a yellow solid. (Yield 40%)

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-87992de327be4e00add2fb1853679525
출처 데이터셋
uspto-grants-2013_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08420635B2

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