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Tetrahydrofuran → (2-Amino-4-fluorophenyl)methanol

HRID 1838057
ノート
印刷プレビュー

反応式

HRID 1838057 の反応式
[NH2:1][C:2]1[CH:10]=[C:9]([F:11])[CH:8]=[CH:7][C:3]=1[C:4](O)=[O:5].C1COCC1.B.C1COCC1>C(O)C>[NH2:1][C:2]1[CH:10]=[C:9]([F:11])[CH:8]=[CH:7][C:3]=1[CH2:4][OH:5]
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 8028TetrahydrofuranHCID 2723981Borane;tetrahydrofuranHCID 27249674-Fluoroanthranilic acid

生成物 1

HCID 12737325(2-Amino-4-fluorophenyl)methanol収率 74.2%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
23 °C

実験手順

To a solution of 2-amino-4-fluorobenzoic acid (3.00 g, 19.3 mmol) and THF (40 mL) at 0° C. under argon, borane-THF complex (1M THF solution, 77.0 mmol) was added dropwise over 30 min. After complete addition, the reaction was warmed to 23° C. After 4 h, the reaction mixture was added slowly (5 min) to ethanol (77 mL). After 20 min, the reaction was concentrated in vacuo, diluted with sat'd NaHCO3 (100 mL), extracted with ethyl acetate (2×100 mL), washed with brine (1×100 mL), and dried (MgSO4). After concentration in vacuo, the residue was purified by passing through a silica gel pad (1:1 ethyl acetate:hexane). Concentration in vacuo afforded 2.02 g of 2-amino-4-fluorobenzyl alcohol as a yellow solid which was sufficiently pure to take on to the next step: 1H NMR (CDCl3) δ 4.54 (br s), 6.28-6.47 (m), 6.93-7.05 (m); 13C NMR (CDCl3) δ 62.7, 101.9 (J=24 Hz), 103.4 (J=21 Hz), 121.5, 130.1 (J=10 Hz), 149.1, 163 (J=360 Hz). MS (EI) 141 (M+), 124, 110. IR (neat) 3500-3000 cm−1.

後処理

  1. additionAfter complete addition
  2. waitAfter 20 min
  3. concentrationthe reaction was concentrated in vacuo
  4. additiondiluted with sat'd NaHCO3 (100 mL)
  5. extractionextracted with ethyl acetate (2×100 mL)
  6. washwashed with brine (1×100 mL)
  7. dry with materialdried (MgSO4)
  8. concentrationAfter concentration in vacuo
  9. customthe residue was purified
  10. concentrationConcentration in vacuo

出典と根拠

ORDレコード
ord-99690f7c5bf84ac5b38aad69d42cbd5e
出典データセット
uspto-grants-2004_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06673784B1

反応ノート

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