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Aluminium lithium hydride → (3-Amino-2-fluorophenyl)methanol

HRID 38682
ノート
印刷プレビュー

反応式

HRID 38682 の反応式
[NH2:1][C:2]1[C:3]([F:11])=[C:4]([CH:8]=[CH:9][CH:10]=1)[C:5](O)=[O:6].[H-].[H-].[H-].[H-].[Li+].[Al+3]>C1COCC1.CCOC(C)=O>[NH2:1][C:2]1[C:3]([F:11])=[C:4]([CH2:5][OH:6])[CH:8]=[CH:9][CH:10]=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

5

反応物 2

HCID 21226445Aluminium lithium hydride3 回HCID 230943433-Amino-2-fluorobenzoic acid

生成物 1

HCID 53249229(3-Amino-2-fluorophenyl)methanol収率 50.1%

試薬・触媒・溶媒 2

HCID 8028Tetrahydrofuran溶媒HCID 8857Ethyl Acetate溶媒

反応条件

温度
0 °C

実験手順

3-amino-2-fluorobenzoic acid (APIN, 250 mg, 1.612 mmol) was dissolved in 10 mL of anhydrous THF under N2 atmosphere. Solution was cooled at 0° C. in an ice-water bath. LiAlH4 (FLUKA, 183 mg, 4.83 mmol) was added. Reaction was stirred under nitrogen at room temperature. After 2 h one equivalent of LiAlH4 (FLUKA, 61 mg, 1.62 mmol) was added to the mixture and reaction was stirred at room temperature overnight. Another equivalent of LiAlH4 (FLUKA, 61 mg, 1.62 mmol) was added. After 5 h The reaction mixture was quenched by adding MeOH. Solvent was evaporated to obtain an orange syrup that was dissolved in EtOAc and partitioned with saturated NaHCO3 (aqueous) (10 mL of saturated solution+15 mL of distilled water). Aqueous phase was extracted with EtOAc, organic layers were combined and dried with MgSO4 (anh), filtered off and concentrated. Crude was purified using silica gel cartridge with linear gradient 0-85% DCM/MeOH to yield the title compound (114 mg, 0.808 mmol, 50.1% yield) as yellow syrup. 1H NMR (300 MHz, DMSO-d6) δ ppm: 6.50-6.85 (m, 3H), 4.95-5.08 (m, 3H), 4.44 (d, 2H).

後処理

  1. customReaction
  2. stirringwas stirred at room temperature overnight
  3. customAfter 5 h The reaction mixture was quenched
  4. additionby adding MeOH
  5. customSolvent was evaporated
  6. customto obtain an orange syrup that
  7. custompartitioned with saturated NaHCO3 (aqueous) (10 mL of saturated solution+15 mL of distilled water)
  8. extractionAqueous phase was extracted with EtOAc, organic layers
  9. dry with materialdried with MgSO4 (anh)
  10. filtrationfiltered off
  11. concentrationconcentrated
  12. customCrude was purified

出典と根拠

ORDレコード
ord-970e1aba485d4c99b3702526307d880f
出典データセット
uspto-grants-2013_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08524750B2

反応ノート

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