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Boron tribromide → 2,6-Dimethyl-4-phenyl-phenol

HRID 2222224
ノート
印刷プレビュー

反応式

HRID 2222224 の反応式
B(Br)(Br)Br.[CH3:5][C:6]1[CH:11]=[C:10]([C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)[CH:9]=[C:8]([CH3:18])[C:7]=1[O:19]C>ClCCl>[CH3:5][C:6]1[CH:11]=[C:10]([C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)[CH:9]=[C:8]([CH3:18])[C:7]=1[OH:19]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 25134Boron tribromideHCID 468699604-Methoxy-3,5-dimethyl-1,1'-biphenyl

生成物 1

HCID 97942002,6-Dimethyl-4-phenyl-phenol収率 98%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

T-butyllithium (1.3M in pentane, 17.9 ml, 23.2 mmol) was added slowly to a solution of 2,6-dimethyl-4-bromo-methoxybenzene (2.5 g, 11.6 mmol) in anhydrous THF (50 ml) at −78° C. under an atmosphere of argon, then after 1 hour a solution of anhydrous zinc chloride (1.6 g, 11.7 mmol) in THF (40 ml) was added by cannula and the clear solution allowed to warm to room temperature and stir for 1 hr. This solution was then added by cannula to iodobenzene (2.37 g, 11.6 mmol) and bis(triphenylphosphine)palladium (II)chloride (81 mg, 116 μmol) in THF (40 ml) and allowed to stir overnight. The reaction was added to 1N HCl (150 ml) and extracted into dichloromethane (2×300 ml). The organic phase was washed with water (150 ml), brine (150 ml) and dried (Na2SO4). The crude product was concentrated and purified by chromatography on silica gel (100 g), eluent 10% dichloromethanelhexanes to give 2,6-dimethyl-4-phenyl-methoxybenzene (2.11 g, 9.9 mmol) in 86% yield. 1H nmr (CDCl3): δ=7.6-7.2 (m, 7H); 3.78 (s, 3H) and 2.37 (s, 6H). Boron tribromide (4.72 g, 19 mmol) was added dropwise to a solution of 2,6-dimethyl-4-phenyl-methoxybenzene (2.35 g, 11.1 mmol) in dichloromethane (45 ml) at −78° C. under argon, then the solution was allowed to warm to room temperature overnight. Ice/water (75 g) was added to quench the reaction, then the reaction was extracted with dichloromethane (2×200 ml). The organic layer was washed with water (50 ml), brine (50 ml) and dried (Na2SO4). Removal of the solvent gave 2,6-dimethyl-4-phenyl-phenol (2.15 g, 10.8 mmol) in 98% yield as a white solid, a single component by TLC Rf (0.13) eluent 4:1 dichloromethane/hexanes and 1H nmr. 1H nmr (CDCl3): δ=7.6-7.2 (m, 7H); 4.70 (s, 1H) and 2.37 (m, 6H).

後処理

  1. customto quench
  2. customthe reaction
  3. extractionthe reaction was extracted with dichloromethane (2×200 ml)
  4. washThe organic layer was washed with water (50 ml), brine (50 ml)
  5. dry with materialdried (Na2SO4)
  6. customRemoval of the solvent

出典と根拠

ORDレコード
ord-8dd6a9984ff34d82ba6bebaa001e8a5b
出典データセット
uspto-grants-2008_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07371755B1

反応ノート

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