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Sodium Iodide → HCID 67015924, 화합물

HRID 1695185
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HRID 1695185 반응식
[CH3:1][O:2][C:3](=[O:12])[C:4]1[CH:9]=[CH:8][C:7]([OH:10])=[C:6]([Cl:11])[CH:5]=1.[Na+].[I-].C([O-])([O-])=O.[K+].[K+].Br[CH2:22][CH:23]1[CH2:25][CH2:24]1>CC(C)=O>[CH3:1][O:2][C:3](=[O:12])[C:4]1[CH:9]=[CH:8][C:7]([O:10][CH2:22][CH:23]2[CH2:25][CH2:24]2)=[C:6]([Cl:11])[CH:5]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 5238Sodium IodideHCID 11430Potassium CarbonateHCID 77580Methyl 3-chloro-4-hydroxybenzoateHCID 81503Bromomethylcyclopropane

생성물 1

HCID 67015924HCID 67015924, 화합물수율 67.7%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

3-Chloro-4-hydroxy-benzoic acid methyl ester (1.1 g, 6.0 mmol, 1.0 eq) was dissolved in acetone (14 mL), NaI (0.45 g, 3.0 mmol, 0.5 eq) and K2CO3 (1.66 g, 12.0 mmol, 2.0 eq) were added ad the mixture was stirred at room temperature for 20 min. (Bromomethyl)cyclopropane (0.53 mL, 5.4 mmol, 0.9 eq) was added, and the mixture was refluxed for 2 days. The solvent was concentrated under reduced pressure, NaOH 10% was added, and the crude was extracted with DCM and dried. The title product (0.88 g, yield 32%) was recovered and used without further purification.

후처리

  1. additionwas added
  2. temperaturethe mixture was refluxed for 2 days
  3. concentrationThe solvent was concentrated under reduced pressure, NaOH 10%
  4. additionwas added
  5. extractionthe crude was extracted with DCM
  6. customdried

출처 및 근거

ORD 기록
ord-86ac654af4d643bba76a5e682b22d56b
출처 데이터셋
uspto-grants-2012_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08163729B2

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