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N-bromobutanimide → 4-Bromo-7-methoxy-2-methoxymethylbenzofuran

HRID 2270119
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HRID 2270119 반응식
[CH3:1][O:2][C:3]1[C:11]2[O:10][C:9]([CH2:12][O:13][CH3:14])=[CH:8][C:7]=2[CH:6]=[CH:5][CH:4]=1.[Br:15]N1C(=O)CCC1=O>C(#N)C>[Br:15][C:6]1[C:7]2[CH:8]=[C:9]([CH2:12][O:13][CH3:14])[O:10][C:11]=2[C:3]([O:2][CH3:1])=[CH:4][CH:5]=1
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참가 물질

4

반응물 2

HCID 67184N-bromobutanimideHCID 184236407-Methoxy-2-methoxymethylbenzofuran

생성물 1

HCID 184236394-Bromo-7-methoxy-2-methoxymethylbenzofuran수율 110.7%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

A solution of 7-methoxy-2-methoxymethylbenzofuran (13.32 g) in acetonitrile (500 ml) was stirred at room temperature. N-bromosuccinimide (11.04 g) was added and stirring continued for 2 days after which the solvent was removed in vacuo. The resulting oil was partitioned between ethyl acetate (100 ml) and sodium metasulfite solution (50 ml), the organic extract washed with more sodium metasulfite solution (2×50 ml), followed by brine (50 ml). The organic layer was separated, dried over magnesium sulphate, filtered and the solvent removed in vacuo to afford the title compound as a yellow oil (18.61 g).

후처리

  1. customafter which the solvent was removed in vacuo
  2. customThe resulting oil was partitioned between ethyl acetate (100 ml) and sodium metasulfite solution (50 ml)
  3. extractionthe organic extract
  4. washwashed with more sodium metasulfite solution (2×50 ml)
  5. customThe organic layer was separated
  6. dry with materialdried over magnesium sulphate
  7. filtrationfiltered
  8. customthe solvent removed in vacuo

출처 및 근거

ORD 기록
ord-539731bc6a884ee399288dab12ae68e7
출처 데이터셋
uspto-grants-2001_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06331556B2

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