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Trimethyl borate → 3-Borono-4-methylbenzoic acid

HRID 2275408
ノート
印刷プレビュー

反応式

HRID 2275408 の反応式
Br[C:2]1[CH:3]=[C:4]([CH:8]=[CH:9][C:10]=1[CH3:11])[C:5]([OH:7])=[O:6].[Li]CCCC.[B:17](OC)([O:20]C)[O:18]C>C1COCC1>[B:17]([C:2]1[CH:3]=[C:4]([CH:8]=[CH:9][C:10]=1[CH3:11])[C:5]([OH:7])=[O:6])([OH:20])[OH:18]
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

5

反応物 3

HCID 8470Trimethyl borateHCID 821303-Bromo-4-methylbenzoic acidHCID 178418339Butyllithium

生成物 1

HCID 189801423-Borono-4-methylbenzoic acid収率 33%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
-78 °C

実験手順

3-Bromo-4-methylbenzoic acid (11.00 g, 51.2 mmol) was dissolved in anhydrous THF (150 ml) under argon in a 500 ml 3-necked round bottom flask fitted with two dropping funnels and argon inlet. The stirred solution was cooled to −78° C. and n-BuLi (1.6M in hexane, 60.7 ml, 97.0 mmol) was added drop wise from a dropping funnel (during 1 h). After completion of the addition, the solution was stirred at −78° C. for another 1 h. To this, B(OMe)3 (17.7 ml, 159.0 mmol) was added slowly from a second dropping funnel. The mixture was stirred 1 h at −78° C. and then warmed up to room temperature overnight. The solvent was evaporated under reduced pressure. The crude product was dissolved in ether and poured into aqueous HCl (1N). The mixture was extracted with ether (3×150 ml), and the combined organic layers were washed with brine, dried over anhydrous MgSO4, filtered, and evaporated to dryness. The crude product was purified using an ISCO system (220 g silica column, hexane/EtOAc gradient and later DCM/MeOH gradient). The impurities washed off in hexane/EtOAc and the pure product eluted in MeOH/DCM (5:95) solvent mixture to give 3.3 g (33% yield) of pure SKC-01-126. 1H NMR (400 MHz, Acetone-d6) δ 12.10 (br s, 1H), 8.16 (s, 1H), 7.90-7.63 (m, 1H), 7.11 (d, J=7.9 Hz, 1H), 2.42 (s, 3H).

後処理

  1. customfitted with two dropping funnels and argon inlet
  2. additionAfter completion of the addition
  3. stirringThe mixture was stirred 1 h at −78° C.
  4. temperaturewarmed up to room temperature overnight
  5. customThe solvent was evaporated under reduced pressure
  6. dissolutionThe crude product was dissolved in ether
  7. additionpoured into aqueous HCl (1N)
  8. extractionThe mixture was extracted with ether (3×150 ml)
  9. washthe combined organic layers were washed with brine
  10. dry with materialdried over anhydrous MgSO4
  11. filtrationfiltered
  12. customevaporated to dryness
  13. customThe crude product was purified
  14. washThe impurities washed off in hexane/EtOAc
  15. washthe pure product eluted in MeOH/DCM (5:95) solvent mixture
  16. customto give 3.3 g (33% yield) of pure SKC-01-126

出典と根拠

ORDレコード
ord-eafc9a89100a425f9a471bcbcbb945b6
出典データセット
uspto-grants-2015_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09127024B2

反応ノート

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