Methanol → HCID 19594690、化合物

HRID 612607ノート

反応式

HRID 612607 の反応式
[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]

参加物

7

反応物 4

HCID 887MethanolHCID 6344DichloromethaneHCID 516892Sodium BicarbonateHCID 11036795HCID 11036795、化合物

生成物 1

HCID 19594690HCID 19594690、化合物

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

反応条件

温度
70 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-09f27f7be92a4133bbd832c4bca3c8a6
出典データセット
uspto-grants-1999_12
特許番号
US06004959

反応ノート

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