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Dichloromethane → HCID 22490886, 화합물

HRID 2180553
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HRID 2180553 반응식
[Br:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][C:11]=1[O:12]C)[CH:8]([CH3:14])[CH:7](C)[CH2:6][CH2:5]2.B(Br)(Br)Br.Cl[CH2:21]Cl>>[Br:1][C:2]1[C:11]([OH:12])=[CH:10][C:9]2[C:8]([CH3:14])([CH3:21])[CH2:7][CH2:6][CH2:5][C:4]=2[CH:3]=1
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참가 물질

4

반응물 3

HCID 6344DichloromethaneHCID 25134Boron tribromideHCID 22490924HCID 22490924, 화합물

생성물 1

HCID 22490886HCID 22490886, 화합물

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온도
0 °C

실험 절차

To 6-bromo-7-methoxy-1,2-dimethyl-1,2,3,4-tetrahydro-naphthalene (Compound A-1 ([U.S. Pat. No. 6,613,917, incorporated herein by reference), 6.34 g, 23.56 mmol) in dichloromethane (10 mL) at −30° C. was added a solution of boron tribromide (1.0 M in dichloromethane, 47 mL, 47 mmol). After warming to 0° C. over 1 h, the reaction mixture was quenched carefully with ice water and extracted with ether. The organic layer was washed successively with water, brine, dried over Na2SO4, and concentrated in vacuo. Purification by flash column chromatography (silica gel, 5% ethyl acetate/hexane) yielded the title compound as a white solid.

후처리

  1. customthe reaction mixture was quenched carefully with ice water
  2. extractionextracted with ether
  3. washThe organic layer was washed successively with water, brine
  4. dry with materialdried over Na2SO4
  5. concentrationconcentrated in vacuo
  6. customPurification by flash column chromatography (silica gel, 5% ethyl acetate/hexane)

출처 및 근거

ORD 기록
ord-94385a19c02848aa995f0a9e4fa356d1
출처 데이터셋
uspto-grants-2005_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06887896B1

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