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Hydrochloric Acid → HCID 19094772、化合物

HRID 1866834
ノート
印刷プレビュー

反応式

HRID 1866834 の反応式
C(=O)([O-])[O-].[K+].[K+].C([O:10][C:11]1[C:16]([CH:17]2[CH2:19][CH2:18]2)=[CH:15][CH:14]=[CH:13][C:12]=1[Br:20])(=O)C.O.Cl>CO>[Br:20][C:12]1[CH:13]=[CH:14][CH:15]=[C:16]([CH:17]2[CH2:18][CH2:19]2)[C:11]=1[OH:10]
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 313Hydrochloric AcidHCID 962WaterHCID 11430Potassium CarbonateHCID 69045518HCID 69045518、化合物

生成物 1

HCID 19094772HCID 19094772、化合物収率 55.4%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

Potassium carbonate (276 mg, 2.00 mmol) was added to a solution of 2-bromo-6-cyclopropylphenyl acetate (316 mg, purity: 80%, 1.00 mmol) in methanol (2 ml), and the mixture was stirred at room temperature for 4 hours. After water (15 ml) and 4M hydrochloric acid (15 ml) were added to the reaction mixture, the mixture was extracted with ethyl acetate. The organic layer was combined, washed with a saturated aqueous NaCl solution, followed by drying with anhydrous sodium sulfate. After the solid was removed by filtration, the filtrate was concentrated to obtain a pale brown oil. This oil was purified by preparative thin layer chromatography (manufactured by Merck Co., Ltd, 1.05744, use of two sheets, development by hexane:ethyl acetate=30:1) to obtain 118 mg of 2-bromo-6-cyclopropylphenol.

後処理

  1. extractionthe mixture was extracted with ethyl acetate
  2. washwashed with a saturated aqueous NaCl solution
  3. dry with materialby drying with anhydrous sodium sulfate
  4. customAfter the solid was removed by filtration
  5. concentrationthe filtrate was concentrated
  6. customto obtain a pale brown oil
  7. customThis oil was purified by preparative thin layer chromatography (manufactured by Merck Co., Ltd, 1.05744, use of two sheets, development by hexane:ethyl acetate=30:1)

出典と根拠

ORDレコード
ord-fb3b1fe3ea1742df8bd4b61096efefa7
出典データセット
uspto-grants-2009_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07629494B2

反応ノート

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