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2,3-Dichloro-5,6-dicyano-1,4-benzoquinone → 9-Bromo-3-chloro-8-methoxy-6,6-dimethyl-5,6-dihydro-benzo[b]carbazol-11-one

HRID 61824
ノート
印刷プレビュー

反応式

HRID 61824 の反応式
[Br:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][C:11]=1[O:12][CH3:13])[C:8]([CH3:15])([CH3:14])[C:7](=O)[CH2:6][CH2:5]2.Cl.[Cl:18][C:19]1[CH:20]=[C:21]([NH:25]N)[CH:22]=[CH:23][CH:24]=1.C(OCC)(=[O:29])C.C(C1C(=O)C(Cl)=C(Cl)C(=O)C=1C#N)#N>C(O)(=O)C.C1COCC1.C1COCC1.C(OCC)C.O>[Br:1][C:2]1[C:11]([O:12][CH3:13])=[CH:10][C:9]2[C:8]([CH3:15])([CH3:14])[C:7]3[NH:25][C:21]4[C:22]([C:6]=3[C:5](=[O:29])[C:4]=2[CH:3]=1)=[CH:23][CH:24]=[C:19]([Cl:18])[CH:20]=4
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

9

反応物 4

HCID 67752,3-Dichloro-5,6-dicyano-1,4-benzoquinoneHCID 8857Ethyl AcetateHCID 75331m-Chlorophenylhydrazine hydrochlorideHCID 545785436-Bromo-7-methoxy-1,1-dimethyl-3,4-dihydronaphthalen-2(1H)-one2 回

生成物 1

HCID 668349559-Bromo-3-chloro-8-methoxy-6,6-dimethyl-5,6-dihydro-benzo[b]carbazol-11-one

試薬・触媒・溶媒 4

HCID 176
Acetic Acid
溶媒
HCID 962Water溶媒
HCID 8028Tetrahydrofuran溶媒
HCID 21868444Ether tetrahydrofuran溶媒

反応条件

温度
90 °C

実験手順

6-Bromo-7-methoxy-1,1-dimethyl-3,4-dihydro-1H-naphthalen-2-one (Compound E1, 0.2 g, 0.71 mmol) and 3-chlorophenylhydrazine hydrochloric acid salt (0.17 g, 1.3 eq.) were dissolved in acetic acid (0.5 mL). Under nitrogen atmosphere, the reaction solution was stirred at 90° C. for 8 hr. After cooling to room temperature, the reaction solution was added with ethyl acetate, washed with water, saturated aqueous solution of sodium hydrogen carbonate and saturated brine and dried over magnesium sulfate. After filtration and concentration under reduced pressure, the residues obtained therefrom were dissolved in THF (3 mL) comprising 10% water, added with DDQ (227 mg, 3 eq.) at room temperature, and the mixture was stirred at room temperature for 2 hr. The reaction solution was added with the mixture liquid of THF/diethyl ether (1:1) and washed with 0.5 N aqueous solution of sodium hydroxide and saturated brine. After drying with sodium sulfate, the mixture was filtered and the resulting residues obtained after concentration under reduced pressure were washed with the mixture liquid of hexane/diethyl ether (1:1) to obtain the title compound (brown powder, 86 mg).

後処理

  1. temperatureAfter cooling to room temperature
  2. washwashed with water, saturated aqueous solution of sodium hydrogen carbonate and saturated brine
  3. dry with materialdried over magnesium sulfate
  4. filtrationAfter filtration and concentration under reduced pressure
  5. customthe residues obtained
  6. stirringthe mixture was stirred at room temperature for 2 hr
  7. washwashed with 0.5 N aqueous solution of sodium hydroxide and saturated brine
  8. dry with materialAfter drying with sodium sulfate
  9. filtrationthe mixture was filtered
  10. customthe resulting residues obtained
  11. concentrationafter concentration under reduced pressure
  12. washwere washed with the mixture liquid of hexane/diethyl ether (1:1)

出典と根拠

ORDレコード
ord-a56d46741b48439aa5aef8419e6a0b34
出典データセット
uspto-grants-2016_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09440922B2

反応ノート

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