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Ethanol → 5-Bromo-2-{3-fluoro-4-[(phenylmethyl)oxy]phenyl}pyridine

HRID 423573
ノート
印刷プレビュー

反応式

HRID 423573 の反応式
[CH2:1]([O:8][C:9]1[CH:14]=[CH:13][C:12](B(O)O)=[CH:11][C:10]=1[F:18])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.Br[C:20]1[CH:25]=[CH:24][C:23]([Br:26])=[CH:22][N:21]=1.C([O-])([O-])=O.[Na+].[Na+].CCO>C1(C)C=CC=CC=1.C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1>[Br:26][C:23]1[CH:24]=[CH:25][C:20]([C:12]2[CH:13]=[CH:14][C:9]([O:8][CH2:1][C:2]3[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=3)=[C:10]([F:18])[CH:11]=2)=[N:21][CH:22]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 702EthanolHCID 10340Sodium CarbonateHCID 693532,5-DibromopyridineHCID 27377884-Benzyloxy-3-fluorophenylboronic Acid

生成物 1

HCID 666732465-Bromo-2-{3-fluoro-4-[(phenylmethyl)oxy]phenyl}pyridine収率 77%

試薬・触媒・溶媒 2

HCID 178418397
HCID 178418397、化合物
触媒
HCID 1140Toluene溶媒

反応条件

温度
90 °C

実験手順

(4-Benzyloxy-3-fluorophenyl)boronic acid (1.06 g, 4.22 mmol) was added to a suspension of 2,5-dibromopyridine (1.0 g, 4.22 mmol) in toluene (8 mL), followed by addition of 2M Na2CO3 (6 mL) and Pd(PPh3)4 (0.15 g, 0.13 mmol) and EtOH (2 mL). The reaction mixture was degassed with N2 and heated at 90° C. overnight. The mixture was cooled to ambient temperature, water was added, and the mixture was extracted with EtOAc. The combined organic extract was washed with brine, dried over Na2SO4, filtered through a pad of silica gel, and the filtrate was concentrated to give a solid, which was recrystallized from MeOH to give 1.16 g (77%) of 5-bromo-2-{3-fluoro-4-[(phenylmethyl)oxy]phenyl}pyridine as a faint yellow solid. 1H NMR (400 MHz, CDCl3): δ 8.69 (d, 1H, J=2.2 Hz), 7.85 (dd, 1H, Ja=8.4 Hz, Jb=2.1 Hz), 7.77 (dd, 1H, Ja=12.4 Hz, Jb=2.1 Hz), 7.67 (d, 1H, J=8.6 Hz), 7.54 (d, 1H, J=8.5 Hz), 7.50-7.30 (m, 5H), 7.07 (t, 1H, J=8.4 Hz), 5.20 (s, 2H); LRMS (ESI), m/z 358/360 (M+H).

後処理

  1. customThe reaction mixture was degassed with N2
  2. temperatureThe mixture was cooled to ambient temperature
  3. additionwater was added
  4. extractionthe mixture was extracted with EtOAc
  5. extractionThe combined organic extract
  6. washwas washed with brine
  7. dry with materialdried over Na2SO4
  8. filtrationfiltered through a pad of silica gel
  9. concentrationthe filtrate was concentrated
  10. customto give a solid, which
  11. customwas recrystallized from MeOH

出典と根拠

ORDレコード
ord-d9dcb8ef6a5f4ae3b5f6bb92c8556051
出典データセット
uspto-grants-2012_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08101634B2

反応ノート

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