N-bromobutanimide → 2-(3-(Bromomethyl)-4-methoxyphenyl)acetic acid

HRID 553295

反応式

HRID 553295 の反応式
[Br:1]N1C(=O)CCC1=O.[CH3:9][O:10][C:11]1[CH:16]=[CH:15][C:14]([CH2:17][C:18]([OH:20])=[O:19])=[CH:13][C:12]=1[CH3:21]>C(Cl)(Cl)Cl.N(C(C)(C)C#N)=NC(C)(C)C#N>[Br:1][CH2:21][C:12]1[CH:13]=[C:14]([CH2:17][C:18]([OH:20])=[O:19])[CH:15]=[CH:16][C:11]=1[O:10][CH3:9]

参加物

5

反応物 2

HCID 67184N-bromobutanimideHCID 1382764-Methoxy-3-methylphenylacetic acid

生成物 1

HCID 671652482-(3-(Bromomethyl)-4-methoxyphenyl)acetic acid収率 96.2%

試薬・触媒・溶媒 2

HCID 6547Azobisisobutyronitrile触媒HCID 6212Chloroform溶媒

実験手順

N-Bromosuccinimide (1.0 g) and 2,2′-azobis(2-methylpropionitrile) (20 mg) were added to a solution of (4-methoxy-3-methyl-phenyl)-acetic acid (1.1 g) in chloroform (25 mL) and heated to reflux for 4 hours. On cooling, the mixture was evaporated, the residue dissolved in ethyl acetate, washed sequentially with 2M aqueous hydrochloric acid (2×50 mL), brine (50 mL), dried (magnesium sulfate) and concentrated to give the subtitle compound as an oil (1.4 g).

後処理

  1. temperatureheated
  2. temperatureto reflux for 4 hours
  3. temperatureOn cooling
  4. customthe mixture was evaporated
  5. dissolutionthe residue dissolved in ethyl acetate
  6. washwashed sequentially with 2M aqueous hydrochloric acid (2×50 mL), brine (50 mL)
  7. dry with materialdried (magnesium sulfate)
  8. concentrationconcentrated

出典と根拠

ORDレコード
ord-8d9af2899a0c4e54b61b9d2a76179eb2
出典データセット
uspto-grants-2011_05
特許番号
US07951954B2

関連ノート

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