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Hydrochloric Acid → HCID 66602549、化合物

HRID 2097472
ノート
印刷プレビュー

反応式

HRID 2097472 の反応式
CO.[Br:3][C:4]1[CH:9]=[CH:8][C:7]([O:10][CH:11]([F:13])[F:12])=[C:6]([O:14]CC2CC2)[CH:5]=1.Cl>O>[Br:3][C:4]1[CH:9]=[CH:8][C:7]([O:10][CH:11]([F:12])[F:13])=[C:6]([OH:14])[CH:5]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 887MethanolHCID 100172571-Bromo-3-cyclopropylmethoxy-4-difluoromethoxybenzene

生成物 1

HCID 66602549HCID 66602549、化合物収率 101.9%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

To 60 ml of methanol solution containing 5.80 g (19.7 mmol) of 4-bromo-2-cyclopropylmethoxy-1-difluoromethoxybenzene (see WO 2004033430) was added 60 ml of conc. hydrochloric acid, and the mixture was refluxed for 5 hours. After completion of the reaction, 60 ml of water was added to the reaction mixture, and the mixture was extracted with diethyl ether. The organic layer after separation was washed with a saturated aqueous solution of sodium chloride, dried over anhydrous sodium sulfate and then concentrated under reduced pressure. The obtained residue was applied to silica gel column chromatography (Eluent; hexane:ethyl acetate=4:1 (V/V)), and the fractions containing the desired compound were concentrated under reduced pressure to obtain 4.80 g of the title compound as a slightly yellowish oil substantially quantitatively.

後処理

  1. temperaturethe mixture was refluxed for 5 hours
  2. additionwas added to the reaction mixture
  3. extractionthe mixture was extracted with diethyl ether
  4. customThe organic layer after separation
  5. washwas washed with a saturated aqueous solution of sodium chloride
  6. dry with materialdried over anhydrous sodium sulfate
  7. concentrationconcentrated under reduced pressure
  8. additionthe fractions containing the desired compound
  9. concentrationwere concentrated under reduced pressure

出典と根拠

ORDレコード
ord-60e6af96f44645dbb01690a0ce83e122
出典データセット
uspto-grants-2013_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08450319B2

反応ノート

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