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2,5-Difluorobenzaldehyde → HCID 23114720、化合物

HRID 2080369
ノート
印刷プレビュー

反応式

HRID 2080369 の反応式
C([Li])CCC.[Si:6]([O:23][CH2:24][C:25]1[CH:26]=[N:27][CH:28]=[C:29]([F:31])[CH:30]=1)([C:19]([CH3:22])([CH3:21])[CH3:20])([C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1)[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1.[F:32][C:33]1[CH:40]=[CH:39][C:38]([F:41])=[CH:37][C:34]=1[CH:35]=[O:36].C(=O)(O)[O-].[Na+]>CCCCCC.O.C(OCC)C>[Si:6]([O:23][CH2:24][C:25]1[CH:30]=[C:29]([F:31])[C:28]([CH:35]([C:34]2[CH:37]=[C:38]([F:41])[CH:39]=[CH:40][C:33]=2[F:32])[OH:36])=[N:27][CH:26]=1)([C:19]([CH3:21])([CH3:22])[CH3:20])([C:13]1[CH:14]=[CH:15][CH:16]=[CH:17][CH:18]=1)[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=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

8

反応物 4

HCID 1376632,5-DifluorobenzaldehydeHCID 516892Sodium BicarbonateHCID 231147533-({[tert-Butyl(diphenyl)silyl]oxy}methyl)-5-fluoropyridineHCID 178418339Butyllithium

生成物 1

HCID 23114720HCID 23114720、化合物収率 79%

試薬・触媒・溶媒 3

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

反応条件

温度
-20 °C

実験手順

At −78° C., a hexane solution (30.0 ml, 46.8 mmol) of n-butyl lithium and N,N,N′N′-tetramethylethylenediamine (7.06 ml, 46.8 mmol) were added sequentially to diethyl ether (250 ml). After stirring at −20° C. for 30 minutes, the reaction mixture was cooled to −78° C., and a diethyl ether (50 ml) solution of 3-(t-butyldiphenylsilyloxymethyl)-5-fluoropyridine (15.5 g, 42.5 mmol) was added thereto. The resulting mixture was stirred at the same temperature for 30 minutes. To the reaction mixture was added 2,5-difluorobenzaldehyde (6.04 g, 42.5 mmol). The resulting mixture was stirred for 2 hours. Water and then, a saturated aqueous solution of sodium bicarbonate were added to the reaction mixture. The resulting mixture was extracted with diethyl ether. The organic layer was dried over anhydrous sodium sulfate and then, filtered. The filtrate was concentrated under reduced pressure. The residue thus obtained was subjected to flash silica gel chromatography. The fraction obtained from the hexane:ethyl acetate=9:1 eluate was concentrated under reduced pressure to give the title compound (17.0 g, 33.5 mmol, 79%) as a colorless oil.

後処理

  1. temperaturethe reaction mixture was cooled to −78° C.
  2. stirringThe resulting mixture was stirred at the same temperature for 30 minutes
  3. stirringThe resulting mixture was stirred for 2 hours
  4. extractionThe resulting mixture was extracted with diethyl ether
  5. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  6. filtrationfiltered
  7. concentrationThe filtrate was concentrated under reduced pressure
  8. customThe residue thus obtained
  9. concentrationethyl acetate=9:1 eluate was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-5af5e15fca2e49a9b291d46987c3d020
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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