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Methanol → (3-Bromo-5-fluorophenyl)methanol

HRID 595981
ノート
印刷プレビュー

反応式

HRID 595981 の反応式
[Br:1][C:2]1[CH:3]=[C:4]([CH:8]=[C:9]([F:11])[CH:10]=1)[C:5](O)=[O:6].B.C1COCC1.CO>C1COCC1>[Br:1][C:2]1[CH:3]=[C:4]([CH2:5][OH:6])[CH:8]=[C:9]([F:11])[CH:10]=1
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 3

HCID 887MethanolHCID 2723981Borane;tetrahydrofuranHCID 27733393-Bromo-5-fluorobenzoic acid

生成物 1

HCID 2769402(3-Bromo-5-fluorophenyl)methanol

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a suspension of 3-bromo-5-fluorobenzoic acid (4.51 g, 20.59 mmol) in THF (41.2 mL) at 0° C., BH3.THF (41.2 mL, 41.2 mmol) was added dropwise over 30 min, the reaction mixture was then allowed to return to room temperature and stirred at room temperature overnight. Methanol (40 mL) was added slowly and stirred at room temperature for 1 h. THF and Methanol was removed in vacuo. The residue was then extracted by EtOAc, and washed with sat.NaHCO3, The organic was dried and concentrated. The crude product was used in next step reaction without purification. LCMS (m/z): 187.2 (MH+−18), 0.66 min. 1H NMR (400 MHz, CDCl3) δ ppm 7.32 (s, 1H), 7.19-7.14 (m, 1H), 7.05 (tdd, J=0.7, 1.5, 9.1 Hz, 1H), 4.70 (br. s., 2H), 1.78 (br. s., 1H).

このページの内容参加物実験手順後処理出典と根拠反応ノート

後処理

  1. customto return to room temperature
  2. stirringstirred at room temperature for 1 h
  3. customTHF and Methanol was removed in vacuo
  4. extractionThe residue was then extracted by EtOAc
  5. washwashed
  6. dry with materialNaHCO3, The organic was dried
  7. concentrationconcentrated
  8. customThe crude product was used in next step reaction without purification
  9. custom187.2 (MH+−18), 0.66 min

出典と根拠

ORDレコード
ord-ce263cb54f1843f780e6e27dc29f5c26
出典データセット
uspto-grants-2016_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09242996B2

反応ノート

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