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Dimethylformamide → 6-fluoro-1H-indazole-5-carbaldehyde

HRID 69136
ノート
印刷プレビュー

反応式

HRID 69136 の反応式
Br[C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][C:10]=1[F:11])[NH:7][N:6]=[CH:5]2.[H-].[Na+].CN([CH:17]=[O:18])C>C1COCC1>[F:11][C:10]1[CH:9]=[C:8]2[C:4]([CH:5]=[N:6][NH:7]2)=[CH:3][C:2]=1[CH:17]=[O: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 6228DimethylformamideHCID 24758Sodium hydrideHCID 468639235-Bromo-6-fluoro-1H-indazole

生成物 1

HCID 579172916-fluoro-1H-indazole-5-carbaldehyde

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒3 回

反応条件

温度
-70 °C

実験手順

A solution of 5-bromo-6-fluoro-1H-indazole (3 g, 13.95 mmol) in THF (10 mL) was added to a suspension of NaH (3.38 g, 141 mmol) in THF (100 mL) over 10 min at 0° C. The RM was cooled to −70° C. then the s-Buli solution (1.4 M, 19 mL) was added slowly over 20 min. It was stirred at this temperature for 45 min. A solution of DMF (6.18 mL, 80 mmol) in THF (10 mL) was added over 15 min at −70° C. and the RM was then warmed up to rt over 1 h 30. The reaction was quenched with 100 mL of 1 N HCl. The RM was extracted twice with EtOAc. Then the organics were joined and washed with brine, dried over Na2SO4 and the solvent was removed. The residue was triturated for 1 h with Et2O. The precipitate formed was filtered off and identified as the desired aldehyde. The filtrate was left in the freezer over night and a second batch of the product was filtered off to afford the title compound as a light yellow solid (tR 0.7 min (conditions 2), MH+=165, 1H-NMR in DMSO-d6: 13.50 (s, 1H); 10.15 (s, 1H); 8.39 (d, 1H); 8.32 (s, 1H); 7.45 (d, 1H)).

後処理

  1. temperaturethe RM was then warmed up to rt over 1 h 30
  2. customThe reaction was quenched with 100 mL of 1 N HCl
  3. extractionThe RM was extracted twice with EtOAc
  4. washwashed with brine
  5. dry with materialdried over Na2SO4
  6. customthe solvent was removed
  7. customThe residue was triturated for 1 h with Et2O
  8. customThe precipitate formed
  9. filtrationwas filtered off
  10. waitThe filtrate was left in the freezer over night
  11. filtrationa second batch of the product was filtered off

出典と根拠

ORDレコード
ord-791dd7a128fa472780a4f13c06961939
出典データセット
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08822468B2

反応ノート

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