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2,5-Difluorobenzaldehyde → 2-[(t-Butyldimethylsilyloxy)methyl]-4-[(2,5-difluorophenyl)hydroxymethyl]-5-methylpyridine

HRID 2080479
ノート
印刷プレビュー

反応式

HRID 2080479 の反応式
C([Li])CCC.Br[C:7]1[C:12]([CH3:13])=[CH:11][N:10]=[C:9]([CH2:14][O:15][Si:16]([C:19]([CH3:22])([CH3:21])[CH3:20])([CH3:18])[CH3:17])[CH:8]=1.[F:23][C:24]1[CH:31]=[CH:30][C:29]([F:32])=[CH:28][C:25]=1[CH:26]=[O:27]>CCCCCC.O.C(OCC)C>[Si:16]([O:15][CH2:14][C:9]1[CH:8]=[C:7]([CH:26]([C:25]2[CH:28]=[C:29]([F:32])[CH:30]=[CH:31][C:24]=2[F:23])[OH:27])[C:12]([CH3:13])=[CH:11][N:10]=1)([C:19]([CH3:22])([CH3:21])[CH3:20])([CH3:18])[CH3:17]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 3

HCID 1376632,5-DifluorobenzaldehydeHCID 231148234-Bromo-2-[(t-butyldimethylsilyloxy)methyl]-5-methylpyridineHCID 178418339Butyllithium

生成物 1

HCID 231147292-[(t-Butyldimethylsilyloxy)methyl]-4-[(2,5-difluorophenyl)hydroxymethyl]-5-methylpyridine収率 74.2%

試薬・触媒・溶媒 3

HCID 962Water溶媒
HCID 3283
Diethyl Ether
溶媒
HCID 8058Hexane溶媒2 回

実験手順

Under an argon atmosphere, n-butyl lithium (a 1.58M hexane solution, 400 μl, 0.632 mmol) was added to a diethyl ether (3 ml) solution of 4-bromo-2-[(t-butyldimethylsilyloxy)methyl]-5-methylpyridine (200 mg, 0.632 mmol) at −78° C. The resulting mixture was stirred for 1 hour. After 2,5-difluorobenzaldehyde (69 μl, 0.632 mmol) was added dropwise, the reaction mixture was stirred for 1 hour. To the reaction mixture were added water and a saturated aqueous solution of sodium bicarbonate, followed by extraction with diethyl ether. The extract was washed with brine. The organic layer thus obtained was dried over magnesium sulfate, and concentrated under reduced pressure. The residue thus obtained was subjected to flash silica gel column chromatography. The fraction obtained from the hexane:ethyl acetate=2:1 eluate was concentrated under reduced pressure to give the title compound (178 mg, 0.469 mmol, 74%) as a white powder.

後処理

  1. stirringthe reaction mixture was stirred for 1 hour
  2. extractiona saturated aqueous solution of sodium bicarbonate, followed by extraction with diethyl ether
  3. washThe extract was washed with brine
  4. customThe organic layer thus obtained
  5. dry with materialwas dried over magnesium sulfate
  6. concentrationconcentrated under reduced pressure
  7. customThe residue thus obtained
  8. concentrationethyl acetate=2:1 eluate was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-016ccfca7b324a2d99ff8b927bbfe0e3
出典データセット
uspto-grants-2011_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07932271B2

反応ノート

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