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Allyl bromide → (+/-)-[6-Fluoro-7-(2-methylphenyl)-2,3-dihydro-1-benzofuran-2-yl]methanol

HRID 2116274
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HRID 2116274 반응식
C[O:2][C:3]1C(C2C=CC=CC=2C)=C(F)C=[CH:7][CH:8]=1.[F:17][C:18]1[CH:19]=[CH:20][CH:21]=[C:22]([OH:31])[C:23]=1[C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][C:25]=1[CH3:30].[H-].[Na+].C(Br)C=C.C(OCC=C)C=C.C(C1C=CC(F)=C(C2C=CC=CC=2C)C=1O)C=C.ClC1C=C(C=CC=1)C(OO)=O.C(=O)([O-])[O-].[K+].[K+]>Br.C1(C)C=C(C)C=C(C)C=1>[F:17][C:18]1[CH:19]=[CH:20][C:21]2[CH2:7][CH:8]([CH2:3][OH:2])[O:31][C:22]=2[C:23]=1[C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][C:25]=1[CH3:30]
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참가 물질

11

반응물 8

HCID 7841Allyl bromideHCID 11194Diallyl etherHCID 11430Potassium CarbonateHCID 24758Sodium hydrideHCID 70297m-Chloroperbenzoic acidHCID 689643673-Allyl-6-fluoro-2'-methylbiphenyl-2-ol2회HCID 689663766-Fluoro-2-methoxy-2'-methyl-biphenyl
HCID 69020361
6-Fluoro-2'-methylbiphenyl-2-ol

생성물 1

HCID 68964662(+/-)-[6-Fluoro-7-(2-methylphenyl)-2,3-dihydro-1-benzofuran-2-yl]methanol수율 80%

시약·촉매·용매 2

HCID 260Hydrogen Bromide용매HCID 7947Mesitylene용매

실험 절차

Treatment of 1-bromo-2-methylbenzene (10.06 g, 58.84 mmol) with (2-fluoro-6-methyoxyphenyl)boronic acid (5.0 g, 29.42 mol tetrakis(triphenylphosphine)palladium(0) (2.5 g, 2.16 mmol), and sodium carbonate (6.2 g, 58.84 mmol) generally according to the procedure described for Intermediate 37 provided 2.35 g (37%) of 6-fluoro-2′-methylbiphenyl-2-yl methyl ether. A solution of 6-fluoro-2′-methylbiphenyl-2-yl methyl ether (2.35 g, 10.86 mmol) in hydrogen bromide (40 mL, 30 wt. % in acetic acid) was heated to 55° C. for 12 h. The reaction mixture was concentrated under in vacuo and the crude residue diluted with ethyl acetate (200 mL). The organic layer was carefully extracted with saturated bicarbonate solution (3×200 mL) was dried (magnesium sulfate), and the solvent was removed in vacuo to provide a crude oil. Treatment of 6-fluoro-2′-methybiphenyl-2-ol (2.17 g, 10.84 mmol) with sodium hydride (0.65 g, 16.26 mmol, 60 wt. %) and allyl bromide (0.96 g, 16.26 mmol), followed by refluxing the resultant allyl ether in mesitylene generally according to the procedure described for Intermediate 8 provided 3-allyl-6-fluoro-2′-methylbiphenyl-2-ol. Treatment of 3-allyl-6-fluoro-2′-methylbiphenyl-2-ol (1.77 g, 7.3 mmol) with 3-chloroperoxybenzoic acid (3.2 g, 10.96 mmol, 77%) followed by potassium carbonate (1.2 g, 8.76 mmol) generally according to the procedure described for Intermediate 9 afforded 1.5 g (80%) of (±)-[6-fluoro-7-(2-methylphenyl)-2,3-dihydro-1-benzofuran-2-yl]methanol. Treatment of (±)-[6-fluoro-7-(2-methylphenyl)-2,3-dihydro-1-benzofuran-2-yl]methanol (1.5 g, 5.81 mmol) with p-toluenesulfonyl chloride (1.66 g, 8.71 mol) generally according to the procedure described for Intermediate 10 gave 2.17 g (90%) of (±)-[6-fluoro-7-(2-methylphenyl)-2,3-dihydro-1-benzofuran-2-yl]methyl 4-methylbenzenesulfonate as a white solid. Treatment of (±)-[6-fluoro-7-(2-methylphenyl)-2,3-dihydro-1-benzofuran-2-yl]methyl 4-methylbenzenesulfonate (0.23 g, 0.56 mmol) with sodium azide (0.23 g, 3.54 mmol) generally according to the procedure described for Intermediate 98 afforded 0.135 g, (86%) of (±)-2-(azidomethyl)-6-fluoro-7-(2-methylphenyl)-2,3-dihydro-1-benzofuran. Treatment of (±)-2-(azidomethyl)-6-fluoro-7-(2-methylphenyl)-2,3-dihydro-1-benzofuran (0.135 g, 0.4 mmol) in tetrahydrofuran (10 mL) with polymer-supported triphenylphosphine (0.30 g, 0.9 mmol) generally according to the procedure described for Example 154 provided 0.11 g (67%) of (±)-{[6-fluoro-7-(2-methylphenyl)-2,3-dihydro-1-benzofuran-2-yl]methyl}amine as a white solid, hydrochloride salt. mp 216-218° C.

후처리

  1. concentrationThe reaction mixture was concentrated under in vacuo
  2. additionthe crude residue diluted with ethyl acetate (200 mL)
  3. extractionThe organic layer was carefully extracted with saturated bicarbonate solution (3×200 mL)
  4. dry with materialwas dried (magnesium sulfate)
  5. customthe solvent was removed in vacuo
  6. customto provide a crude oil

출처 및 근거

ORD 기록
ord-94ab92a983ac49208a5e22ea86ba19d4
출처 데이터셋
uspto-grants-2008_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07435837B2

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