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2-Bromobenzaldehyde → 1-(2-Bromophenyl)-2,2,2-trifluoroethan-1-ol

HRID 1518119
ノート
印刷プレビュー

反応式

HRID 1518119 の反応式
[Br:1][C:2]1[CH:9]=[CH:8][CH:7]=[CH:6][C:3]=1[CH:4]=[O:5].C[Si]([C:14]([F:17])([F:16])[F:15])(C)C>O.[F-].C([N+](CCCC)(CCCC)CCCC)CCC.Cl>[Br:1][C:2]1[CH:9]=[CH:8][CH:7]=[CH:6][C:3]=1[CH:4]([OH:5])[C:14]([F:17])([F:16])[F:15]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 811292-BromobenzaldehydeHCID 552549(Trifluoromethyl)trimethylsilane

生成物 1

HCID 575823691-(2-Bromophenyl)-2,2,2-trifluoroethan-1-ol収率 72%

試薬・触媒・溶媒 2

HCID 162116731-Butanaminium, N,N,N-tributyl-, fluoride, hydrate触媒HCID 313Hydrochloric Acid溶媒

実験手順

The title compound was prepared by an adaptation of the method described in Xue, Y. et al. (Bioorg. Med. Chem. 2007, 15, 2156-2166). Tetrabutylammonium fluoride hydrate (0.05 eq., 131 mg, 0.050 mmol) was placed in a 40 mL vial equipped with a magnetic stir bar, and the vial was evacuated and backflushed with Ar. Dry THF (25 mL) was added via syringe, and 2-bromobenzaldehyde (1.16 mL, 10.0 mmol) and trimethylsilyltrifluoromethane (1.3 eq., 1.90 mL, 13.0 mmol) were sequentially added via syringe. The reaction was stirred at RT for 16 h, and additional CF3 TMS (1 mL) was added. After stirring for 2 h, the reaction was poured into 3 M aq HCl (30 mL) and stirred at RT for 2 h. The reaction mixture was extracted three times with DCM (30 mL), and the combined organic extracts were dried over anhydrous MgSO4, filtered, and the solvent removed under reduced pressure, yielding 1.83 g (72%) of the title compound. 1H-NMR (400 MHz, CDCl3) δ: 7.69 (d, J=7.8 Hz, 1H), 7.60 (dd, J=8.1, 1.3 Hz, 1H), 7.40 (td, J=7.6, 1.1 Hz, 1H), 7.27 (td, J=7.7, 1.8 Hz, 1H), 5.56-5.68 (m, 1H), 2.77 (d, J=4.8 Hz, 1H).

後処理

  1. customThe title compound was prepared by an adaptation of the method
  2. customvial equipped with a magnetic stir bar
  3. customthe vial was evacuated
  4. additionDry THF (25 mL) was added via syringe
  5. stirringAfter stirring for 2 h
  6. stirringstirred at RT for 2 h
  7. extractionThe reaction mixture was extracted three times with DCM (30 mL)
  8. dry with materialthe combined organic extracts were dried over anhydrous MgSO4
  9. filtrationfiltered
  10. customthe solvent removed under reduced pressure

出典と根拠

ORDレコード
ord-25de0d8e9834451ba92fd2ec7b2351a8
出典データセット
uspto-grants-2012_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08232409B2

反応ノート

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