Boron tribromide → HCID 18624168、化合物

HRID 1860689ノート

反応式

HRID 1860689 の反応式
[Br:1][C:2]1[CH:7]=[C:6]([O:8]C)[CH:5]=[CH:4][C:3]=1[CH2:10][C:11]([CH3:19])([CH3:18])[CH2:12][C:13]([O:15][CH2:16][CH3:17])=[O:14].B(Br)(Br)Br>C(Cl)Cl>[Br:1][C:2]1[CH:7]=[C:6]([OH:8])[CH:5]=[CH:4][C:3]=1[CH2:10][C:11]([CH3:18])([CH3:19])[CH2:12][C:13]([O:15][CH2:16][CH3:17])=[O:14]

参加物

4

反応物 2

HCID 25134Boron tribromideHCID 18624146HCID 18624146、化合物

生成物 1

HCID 18624168HCID 18624168、化合物収率 93%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

反応条件

温度
0 °C

実験手順

Ethyl 4-(2-bromo-4-methoxyphenyl)-3,3-dimethylbutanoate (4.5 g, 13.7 mmoles) was dissolved in methylene chloride (60 mL) and was cooled to 0° C. and 1M boron tribromide in methylene chloride (27.0 mL) was added. The mixture was stirred at 0° C. for one hour under nitrogen atmosphere. The reaction mixture was quenched with ethanol (60.0 mL) and was warmed to room temperature and was stirred at room temperature for 1 hour. The solvents were removed under reduced pressure and residue was dissolved in ethyl acetate and was washed with a saturated solution of sodium bicarbonate and water, dried (Na2SO4) and concentrated to yield 4.0 g (93%) of desired product. NMR spectrum of the product was consistent for the proposed structure.

後処理

  1. customThe reaction mixture was quenched with ethanol (60.0 mL)
  2. temperaturewas warmed to room temperature
  3. stirringwas stirred at room temperature for 1 hour
  4. customThe solvents were removed under reduced pressure and residue
  5. dissolutionwas dissolved in ethyl acetate
  6. washwas washed with a saturated solution of sodium bicarbonate and water
  7. dry with materialdried (Na2SO4)
  8. concentrationconcentrated

出典と根拠

ORDレコード
ord-8e94f4b6452247f398589c799bf78d4d
出典データセット
uspto-grants-2003_03
特許番号
US06531494B1

反応ノート

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