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

HRID 1442479

반응식

HRID 1442479 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 684205954-Benzyloxy-2-chloro-benzoic acid ethyl ester수율 86.9%

시약·촉매·용매 1

HCID 6569Methyl Ethyl Ketone용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-effc506ca556489ca6822db551cfe537
출처 데이터셋
uspto-grants-2010_02
특허 번호
US07658979B2

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