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

HRID 1282034
ノート
印刷プレビュー

反応式

HRID 1282034 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

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

生成物 1

HCID 184236394-Bromo-7-methoxy-2-methoxymethylbenzofuran収率 110.7%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-182dc90767a541df9133e751e78b9743
出典データセット
uspto-grants-2002_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06455561B1

反応ノート

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