Benzyl Bromide → 4-Benzyloxy-2-chloro-benzoic acid ethyl ester

HRID 1442479

反応式

HRID 1442479 の反応式
[CH2:1]([O:3][C:4](=[O:13])[C:5]1[CH:10]=[CH:9][C:8]([OH:11])=[CH:7][C:6]=1[Cl:12])[CH3:2].C(=O)([O-])[O-].[K+].[K+].Br[CH2:21][C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1>C(C(C)=O)C>[CH2:1]([O:3][C:4](=[O:13])[C:5]1[CH:10]=[CH:9][C:8]([O:11][CH2:21][C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=2)=[CH:7][C:6]=1[Cl:12])[CH3:2]

参加物

5

反応物 3

HCID 7498Benzyl BromideHCID 11430Potassium CarbonateHCID 19981058Ethyl 2-chloro-4-hydroxybenzoate

生成物 1

HCID 684205954-Benzyloxy-2-chloro-benzoic acid ethyl ester収率 86.9%

試薬・触媒・溶媒 1

HCID 6569Methyl Ethyl Ketone溶媒

実験手順

16.76 g (83.5 mmol) of 2-chloro-4-hydroxy-benzoic acid ethyl ester and 23.1 g (167 mmol) of potassium carbonate were added to 100 mL of methyl ethyl ketone followed by the addition of 17.1 g (100 mmol) of bromomethylbenzene while stirring. After refluxing for 28 hours, the mixture was cooled and filtered. The filtrate was concentrated and the residue was purified by silica gel column chromatography to obtain 21.1 g of a light yellow solid.

後処理

  1. temperatureAfter refluxing for 28 hours
  2. temperaturethe mixture was cooled
  3. filtrationfiltered
  4. concentrationThe filtrate was concentrated
  5. customthe residue was purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-effc506ca556489ca6822db551cfe537
出典データセット
uspto-grants-2010_02
特許番号
US07658979B2

関連ノート

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