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Methyl iodide → 5-Methyl-4,5,6,7-tetrahydrothiazolo(5,4-c)pyridine

HRID 546388
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HRID 546388 반응식
[N:1]1[C:9]2[CH:8]=[CH:7][N:6]=[CH:5][C:4]=2[S:3][CH:2]=1.[CH3:10]I>CN(C)C=O>[CH3:10][N:6]1[CH2:7][CH2:8][C:9]2[N:1]=[CH:2][S:3][C:4]=2[CH2:5]1
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참가 물질

4

반응물 2

HCID 6328Methyl iodideHCID 14666228Thiazolo[5,4-c]pyridine

생성물 1

HCID 111864405-Methyl-4,5,6,7-tetrahydrothiazolo(5,4-c)pyridine

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

Thiazolo[5,4-c]pyridine (1.61 g) was dissolved in N,N-dimethylformamide (50 ml), and to the solution methyl iodide (1.50 ml) was added, the resultant mixture was stirred at 80° C. for 4 hours. The reaction mixture was concentrated under reduced pressure, and the residue was dissolved in methanol (100 ml), sodium borohydride (1.53 g) was added, and the resultant mixture was stirred at room temperature for 1 hour. The reaction mixture was concentrated under reduced pressure, and a saturated aqueous solution of potassium carbonate and ether were added to the residue to separate an organic layer. The organic layer was dried over anhydrous sodium sulfate, and the solvent was distilled off under reduced pressure. The residue was purified by column chromatography on silica gel (dichloromethane:methanol 25:1) to obtain the title compound (1.28 g) as a pale yellow oil.

후처리

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. dissolutionthe residue was dissolved in methanol (100 ml)
  3. additionsodium borohydride (1.53 g) was added
  4. concentrationThe reaction mixture was concentrated under reduced pressure
  5. additiona saturated aqueous solution of potassium carbonate and ether were added to the residue
  6. customto separate an organic layer
  7. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  8. distillationthe solvent was distilled off under reduced pressure
  9. customThe residue was purified by column chromatography on silica gel (dichloromethane:methanol 25:1)

출처 및 근거

ORD 기록
ord-bdedc9fc084f42eab05fab5db8c699ea
출처 데이터셋
uspto-grants-2011_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07935824B2

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