Hydrochloric Acid → HCID 17989091、化合物

HRID 1443281ノート

反応式

HRID 1443281 の反応式
[F:1][C:2]1[C:7]([CH3:8])=[CH:6][CH:5]=[C:4](F)[C:3]=1[O:10][CH3:11].C[Si](C)(C)[N-][Si](C)(C)C.[K+].[C:22](#[N:26])[CH:23]([CH3:25])[CH3:24].Cl>C1(C)C=CC=CC=1>[F:1][C:2]1[C:3]([O:10][CH3:11])=[C:4]([C:23]([CH3:25])([CH3:24])[C:22]#[N:26])[CH:5]=[CH:6][C:7]=1[CH3:8]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 6559IsobutyronitrileHCID 27741352,6-Difluoro-3-methylanisoleHCID 3251421Potassium bis(trimethylsilyl)amide

生成物 1

HCID 17989091HCID 17989091、化合物収率 54.4%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒2 回

実験手順

14.48 g (91.56 mmol) of 2,6-difluoro-3-methylanisole is dissolved in 800 ml of toluene. After 272.2 ml (137.35 mmol) of a 0.5 molar solution of potassium hexamethyl disilazide in toluene is added, 25.31 g (366.26 mmol) of isobutyronitrile is added in drops. The batch is stirred for 10 days at room temperature and then added to a 1 M HCl solution. After being extracted three times with methyl tert-butyl ether, the combined organic extracts are washed with saturated NaCl solution and dried. After spinning-in and chromatography on silica gel (mobile solvent: ethyl acetate/hexane), 10.32 g (49.5%) of the desired compound is obtained.

後処理

  1. extractionAfter being extracted three times with methyl tert-butyl ether
  2. washthe combined organic extracts are washed with saturated NaCl solution
  3. customdried

出典と根拠

ORDレコード
ord-be6e7a18a0434fddb6fcd99ccec96808
出典データセット
uspto-grants-2010_02
特許番号
US07659297B2

反応ノート

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