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1,1-Dibromoethane → HCID 69031119, 화합물

HRID 1868608
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HRID 1868608 반응식
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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 112011,1-DibromoethaneHCID 11430Potassium CarbonateHCID 58209852HCID 58209852, 화합물2회

생성물 1

HCID 69031119HCID 69031119, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-75660f8642944b1aad88a5f44b92adc6
출처 데이터셋
uspto-grants-2009_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07635779B2

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