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Boron tribromide → Methyl 2-ethyl-4-hydroxy-3-methylbenzoate

HRID 388785
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HRID 388785 반응식
[CH2:1]([C:3]1[C:12]([CH3:13])=[C:11]([O:14]C)[CH:10]=[CH:9][C:4]=1[C:5]([O:7][CH3:8])=[O:6])[CH3:2].B(Br)(Br)Br>C(Cl)Cl>[CH2:1]([C:3]1[C:12]([CH3:13])=[C:11]([OH:14])[CH:10]=[CH:9][C:4]=1[C:5]([O:7][CH3:8])=[O:6])[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 25134Boron tribromideHCID 58298861HCID 58298861, 화합물

생성물 1

HCID 58298869Methyl 2-ethyl-4-hydroxy-3-methylbenzoate수율 100.8%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

2.0 g of methyl 2-ethyl-4-methoxy-3-methylbenzoate are dissolved in 50 ml of DCM in a 100 ml round-bottomed flask, and BBr3 is carefully added dropwise at 0° C. The mixture is left to stir at RT for 4 hours. The solvent is distilled off in vacuo, methanol is carefully added to the residue at 0° C., and the mixture is evaporated again in a rotary evaporator. This operation is repeated a further twice, giving 1.88 g of methyl 2-ethyl-4-hydroxy-3-methylbenzoate as oil, which is employed for the next step without further purification; MS-FAB (M+H+)=195,2; Rf (polar method): 1.96 min.

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후처리

  1. waitThe mixture is left
  2. distillationThe solvent is distilled off in vacuo, methanol
  3. additionis carefully added to the residue at 0° C.
  4. customthe mixture is evaporated again in a rotary evaporator

출처 및 근거

ORD 기록
ord-0d8ce31302db43a3bd50894d02318790
출처 데이터셋
uspto-grants-2013_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08377975B2

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