Benzyl Bromide → HCID 501233, 화합물

HRID 1829733노트

반응식

HRID 1829733 반응식
[SH:1][C:2]1[C:7]([OH:8])=[CH:6][CH:5]=[CH:4][N:3]=1.C(=O)([O-])[O-].[K+].[K+].[CH2:15](Br)[C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1>CC(=O)CC>[C:16]1([CH2:15][S:1][C:2]2[C:7]([OH:8])=[CH:6][CH:5]=[CH:4][N:3]=2)[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1

참가 물질

5

반응물 3

HCID 7498Benzyl BromideHCID 11430Potassium CarbonateHCID 178516238HCID 178516238, 화합물

생성물 1

HCID 501233HCID 501233, 화합물수율 65.7%

시약·촉매·용매 1

HCID 6569Methyl Ethyl Ketone용매

실험 절차

To a mixture of 10.0 g of 2-mercapto-3-pyridinol, 11.0 g of potassium carbonate and 100 mL of 2-butanone was added dropwise with stirring, 13.3 g of benzyl bromide. After stirring at 22° C. for two hours, the mixture was heated to reflux for thirty minutes. The reaction mixture was concentrated under reduced pressure, the residue treated with water, and the mixture brought to pH 6 by the addition of acetic acid. The crude product was filtered and recrystallized from toluene to give 11.1 g of the title compound as a grey crystalline solid, mp 103–104° C. The structure of the product was confirmed by its 1H nmr and mass spectra.

후처리

  1. additionwas added dropwise
  2. stirringAfter stirring at 22° C. for two hours
  3. temperaturethe mixture was heated
  4. temperatureto reflux for thirty minutes
  5. concentrationThe reaction mixture was concentrated under reduced pressure
  6. additionthe residue treated with water
  7. additionthe mixture brought to pH 6 by the addition of acetic acid
  8. filtrationThe crude product was filtered
  9. customrecrystallized from toluene

출처 및 근거

ORD 기록
ord-997956b4e4d94a9bb1e879853d7bf065
출처 데이터셋
uspto-grants-2006_06
특허 번호
US07064139B2

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