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Dimethylformamide → 2-Chloro-6-methoxypyridine-3-carbaldehyde

HRID 1474488
ノート
印刷プレビュー

反応式

HRID 1474488 の反応式
Br[C:2]1[C:3]([Cl:10])=[N:4][C:5]([O:8][CH3:9])=[CH:6][CH:7]=1.C([Li])CCC.CN([CH:19]=[O:20])C.O.[Cl-].[NH4+]>C1(C)C=CC=CC=1>[Cl:10][C:3]1[C:2]([CH:19]=[O:20])=[CH:7][CH:6]=[C:5]([O:8][CH3:9])[N:4]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 6228DimethylformamideHCID 467387833-Bromo-2-chloro-6-methoxypyridineHCID 57429219Ammonium chloride monohydrateHCID 178418339Butyllithium

生成物 1

HCID 133826382-Chloro-6-methoxypyridine-3-carbaldehyde

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

The 3-bromo-2-chloro-6-methoxy-pyridine (0.50 g, 2.26 mmol) obtained in (19-1) above was dissolved in toluene (dehydrated) (11 mL), and thereafter, n-butyllithium (1.46 mL, 2.3 mmol, 1.57 mmol/L hexane solution) was added dropwise to the solution at −78° C. in an argon atmosphere. The obtained mixture was stirred at the same temperature as described above for 30 minutes, and DMF (1.0 mL) was then added to the reaction solution. The obtained mixture was further stirred for 30 minutes. Thereafter, a saturated ammonium chloride water (20 mL) was slowly added to the reaction solution, and the temperature of the mixture was then increased to room temperature. The mixture was extracted with diethyl ether (20 mL) twice, and organic layers were gathered. The resultant was dried over anhydrous sodium sulfate and was then filtrated, followed by vacuum concentration. The obtained residue was purified by silica gel column chromatography (SiO2 30 g, hexane:ethyl acetate=95:5 to 80:20), so as to obtain 180 mg of 2-chloro-6-methoxy-3-pyridinecarboxaldehyde.

後処理

  1. additionwas then added to the reaction solution
  2. stirringThe obtained mixture was further stirred for 30 minutes
  3. extractionThe mixture was extracted with diethyl ether (20 mL) twice
  4. dry with materialThe resultant was dried over anhydrous sodium sulfate
  5. filtrationwas then filtrated
  6. concentrationfollowed by vacuum concentration
  7. customThe obtained residue was purified by silica gel column chromatography (SiO2 30 g, hexane:ethyl acetate=95:5 to 80:20)

出典と根拠

ORDレコード
ord-94e3901d239749a8829f6ebe7111c9ce
出典データセット
uspto-grants-2015_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09018238B2

反応ノート

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