Boron tribromide → HCID 18624168, 화합물

HRID 1860689노트

반응식

HRID 1860689 반응식
[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]

참가 물질

4

반응물 2

HCID 25134Boron tribromideHCID 18624146HCID 18624146, 화합물

생성물 1

HCID 18624168HCID 18624168, 화합물수율 93%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

반응 조건

온도
0 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-8e94f4b6452247f398589c799bf78d4d
출처 데이터셋
uspto-grants-2003_03
특허 번호
US06531494B1

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