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Dimethylformamide → 55745-99-8

HRID 926998
ノート
印刷プレビュー

反応式

HRID 926998 の反応式
Br[C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[S:8][CH2:7][CH2:6][CH2:5]2.C([Li])CCC.CCCCCC.CN([CH:26]=[O:27])C.[Cl-].[NH4+]>C1COCC1>[S:8]1[C:9]2[C:4](=[CH:3][C:2]([CH:26]=[O:27])=[CH:11][CH:10]=2)[CH2:5][CH2:6][CH2:7]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 25517Ammonium ChlorideHCID 197020766-bromo-3,4-dihydro-2H-1-benzothiopyranHCID 178418244HCID 178418244、化合物

生成物 1

HCID 5366560555745-99-8

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

6-Bromo-thiochromane (1.00 g) was dissolved in THF (15.0 mL), added dropwise with 2.69 mol/L n-butyl lithium/hexane solution (3.24 mL) at −78° C., and stirred for 1 hour at the same temperature. After adding DMF (0.71 mL) at the same temperature, it was stirred for 16 hours while raising the temperature to room temperature. A saturated aqueous solution of ammonium chloride was added, and after extraction with ethyl acetate, the organic layer was washed with saturated brine. After drying over anhydrous sodium sulfate, the solvent was evaporated under reduced pressure and the residues were purified by silica gel column chromatography (2 to 15% ethyl acetate/hexane) to obtain the title compound (342 mg) as a colorless oil.

後処理

  1. stirringwas stirred for 16 hours
  2. extractionafter extraction with ethyl acetate
  3. washthe organic layer was washed with saturated brine
  4. dry with materialAfter drying over anhydrous sodium sulfate
  5. customthe solvent was evaporated under reduced pressure
  6. customthe residues were purified by silica gel column chromatography (2 to 15% ethyl acetate/hexane)

出典と根拠

ORDレコード
ord-24ffe5624ac74a2e85ec8d5131567a94
出典データセット
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09290440B2

反応ノート

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