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1,1-Dibromoethane → HCID 69031119、化合物

HRID 1868608
ノート
印刷プレビュー

反応式

HRID 1868608 の反応式
C(=O)([O-])[O-].[K+].[K+].[CH2:7]([O:14][C:15]1[CH:16]=[C:17]([CH:30]=[C:31]([O:33][CH2:34][C:35]2[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=2)[CH:32]=1)[C:18]1[O:19][C:20]2[C:25]([C:26](=[O:28])[CH:27]=1)=[CH:24][CH:23]=[C:22]([OH:29])[CH:21]=2)[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1.[Br:41][CH:42](Br)[CH3:43]>CN(C)C=O>[Br:41][CH2:42][CH2:43][O:29][C:22]1[CH:21]=[C:20]2[C:25]([C:26](=[O:28])[CH:27]=[C:18]([C:17]3[CH:16]=[C:15]([O:14][CH2:7][C:8]4[CH:9]=[CH:10][CH:11]=[CH:12][CH:13]=4)[CH:32]=[C:31]([O:33][CH2:34][C:35]4[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=4)[CH:30]=3)[O:19]2)=[CH:24][CH:23]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 112011,1-DibromoethaneHCID 11430Potassium CarbonateHCID 58209852HCID 58209852、化合物2 回

生成物 1

HCID 69031119HCID 69031119、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

Potassium carbonate (2.76 g, 20 mmol) was added to a stirred solution of 3′,5′-dibenzyloxy-7-hydroxy-flavone, 22 (2.25 g, 5 mmol) in dry dimethyl formamide (120 mL). After the mixture was stirred for 30 min, dibromo ethane (5 mL, 58 mmol) was added and the resultant was stirred at room temperature for 12 h. Reaction mixture was filtered through celite, concentrated under reduced pressure and extracted with chloroform. The extract was washed with water, dried over sodium sulphate, filtered and concentrated in vacuo. The residue was purified by column chromatography to afford 56.

後処理

  1. stirringthe resultant was stirred at room temperature for 12 h
  2. customReaction mixture
  3. filtrationwas filtered through celite
  4. concentrationconcentrated under reduced pressure
  5. extractionextracted with chloroform
  6. washThe extract was washed with water
  7. dry with materialdried over sodium sulphate
  8. filtrationfiltered
  9. concentrationconcentrated in vacuo
  10. customThe residue was purified by column chromatography

出典と根拠

ORDレコード
ord-75660f8642944b1aad88a5f44b92adc6
出典データセット
uspto-grants-2009_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07635779B2

反応ノート

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