Methanol → HCID 19594690, 화합물

HRID 612607노트

반응식

HRID 612607 반응식
[CH2:1]([N:3]([CH2:28][CH3:29])[CH2:4][CH2:5][O:6][C:7]1[CH:19]=[CH:18][CH:17]=[C:16]2[C:8]=1[C:9]1[C:10]([O:26][CH3:27])=[CH:11][C:12]([O:24][CH3:25])=[C:13]([N+:21]([O-])=O)[C:14]=1[C:15]2=[O:20])[CH3:2].C(=O)(O)[O-].[Na+].CO.C(Cl)[Cl:38]>C(O)C.O>[ClH:38].[NH2:21][C:13]1[C:14]2[C:15](=[O:20])[C:16]3[C:8](=[C:7]([O:6][CH2:5][CH2:4][N:3]([CH2:28][CH3:29])[CH2:1][CH3:2])[CH:19]=[CH:18][CH:17]=3)[C:9]=2[C:10]([O:26][CH3:27])=[CH:11][C:12]=1[O:24][CH3:25]

참가 물질

7

반응물 4

HCID 887MethanolHCID 6344DichloromethaneHCID 516892Sodium BicarbonateHCID 11036795HCID 11036795, 화합물

생성물 1

HCID 19594690HCID 19594690, 화합물

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

반응 조건

온도
70 °C

실험 절차

Prepare a mixture of 5-(2-diethylamino-ethoxy)-2,4-dimethoxy-1-nitro-fluoren-9-one (0.08 g, 0.18 mmole) and stannous chloride dihydrate (SnCl2.2H2O, 0.80 g, 3.5 mmole) in 20 mL ethanol. Heat at 70° C. under argon overnight. Dilute with about 60 mL water and make slightly basic by addition of 5% sodium bicarbonate. Extract the precipitate with ethyl acetate and dry over magnesium sulfate. Filter and evaporate the solvent. Make acidic (to pH=2) with 5% hydrochloric acid and extract the organics. Make the aqueous phase basic (to pH=8) and extract with methylene chloride. Dry over magnesium sulfate. Filter and evaporate the solvent to obtain a red oil. Chromatron with 7% methanol in methylene choride and condense under high vacuum to obtain the free base of the title compound (0.48 g). m.p. 208°-210° C.

후처리

  1. customPrepare
  2. extractionExtract the precipitate with ethyl acetate
  3. dry with materialdry over magnesium sulfate
  4. filtrationFilter
  5. customevaporate the solvent
  6. extractionextract the organics
  7. extractionextract with methylene chloride
  8. dry with materialDry over magnesium sulfate
  9. filtrationFilter
  10. customevaporate the solvent
  11. customto obtain a red oil

출처 및 근거

ORD 기록
ord-09f27f7be92a4133bbd832c4bca3c8a6
출처 데이터셋
uspto-grants-1999_12
특허 번호
US06004959

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