Iodine → HCID 57517776、化合物

HRID 601774

反応式

HRID 601774 の反応式
[Mg].Br[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[O:9][CH2:10][CH3:11].II.[CH3:14][O:15][C:16]1[CH:17]=[C:18]2[C:22](=[CH:23][CH:24]=1)[NH:21][C:20](=[O:25])[C:19]2=[O:26]>C(OCC)C.C1COCC1>[CH2:10]([O:9][C:4]1[CH:5]=[CH:6][CH:7]=[CH:8][C:3]=1[C:19]1([OH:26])[C:18]2[C:22](=[CH:23][CH:24]=[C:16]([O:15][CH3:14])[CH:17]=2)[NH:21][C:20]1=[O:25])[CH3:11]

参加物

7

反応物 4

HCID 807IodineHCID 383335-MethoxyisatinHCID 685002-Bromophenetole2 回HCID 5462224Magnesium

生成物 1

HCID 57517776HCID 57517776、化合物

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒2 回HCID 8028Tetrahydrofuran溶媒

実験手順

40 g (1.65 mol) of magnesium chips and 5% of the total amount of the 2-bromo-1-ethoxy benzene were added to 100 ml diethyl ether and after adding a few crystals iodine the mixture was carefully heated to initiate the reaction. To the refluxing mixture the remaining amount of 203 ml (1.65 mol) 2-bromo-1-ethoxy benzene, dissolved in 450 ml diethyl ether, was added slowly to maintain the reaction. Then 75 g (0.41 mol) of 5-methoxyisatine, suspended in 750 ml THF, were added to the cooled reaction mixture. After stirring the reaction mixture for 30 minutes at ambient temperature, the mixture was poured into an ice/aqueous NH4Cl mixture. The aqueous phase was extracted with ethyl acetate several times and the combined organic phase was washed with H2O, dried over magnesium sulfate and the solvent was removed in vacuo.

後処理

  1. temperaturewas carefully heated
  2. customthe reaction
  3. additionwas added slowly
  4. temperatureto maintain
  5. customthe reaction
  6. additionwere added to the cooled reaction mixture
  7. extractionThe aqueous phase was extracted with ethyl acetate several times
  8. washthe combined organic phase was washed with H2O
  9. dry with materialdried over magnesium sulfate
  10. customthe solvent was removed in vacuo

出典と根拠

ORDレコード
ord-5bd7c6f166cd45e2b626c0b715b50b18
出典データセット
uspto-grants-2011_03
特許番号
US07902379B2

関連ノート

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