Triethylamine → 2-(2-Phthalimidoethylthio)pyridine

HRID 6084

반응식

HRID 6084 반응식
C(N(CC)CC)C.[SH:8][C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][N:10]=1.Br[CH2:16][CH2:17][N:18]1[C:22](=[O:23])[C:21]2=[CH:24][CH:25]=[CH:26][CH:27]=[C:20]2[C:19]1=[O:28]>C(O)C>[C:19]1(=[O:28])[N:18]([CH2:17][CH2:16][S:8][C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][N:10]=2)[C:22](=[O:23])[C:21]2=[CH:24][CH:25]=[CH:26][CH:27]=[C:20]12

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 113251H-Isoindole-1,3(2H)-dione, 2-(2-bromoethyl)-HCID 178418616HCID 178418616, 화합물

생성물 1

HCID 152314802-(2-Phthalimidoethylthio)pyridine수율 46.9%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

Triethylamine [12.54 ml (90 mmol)] was added to a suspension of 6.67 g (60 mmol) of 2-mercaptopyridine and 15.24 g (60 mmol) of N-(2-bromoethyl)phthalimide in 200 ml of ethanol and stirred at room temperature for 24 hours. The mixture was heated under reflux for 2 hours. The solvent was distilled off, chloroform was added to the residue, and the mixture was washed with water and dried over anhydrous magnesium sulfate. The solvent was distilled off and the residue was purified by column chromatography (eluent: ethyl acetate/n-hexane=1:2) to obtain 8.00 g of the desired compound (46.9%, colorless crystals).

후처리

  1. temperatureThe mixture was heated
  2. temperatureunder reflux for 2 hours
  3. distillationThe solvent was distilled off
  4. additionchloroform was added to the residue
  5. washthe mixture was washed with water
  6. dry with materialdried over anhydrous magnesium sulfate
  7. distillationThe solvent was distilled off
  8. customthe residue was purified by column chromatography (eluent: ethyl acetate/n-hexane=1:2)

출처 및 근거

ORD 기록
ord-515189e1fb57456dae58a0ec857392d2
출처 데이터셋
uspto-grants-1993_09
특허 번호
US05246948

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