HCID 9998883, 화합물 → HCID 3000382, 화합물

HRID 1033003노트

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HRID 1033003 반응식
C([S:5][C:6]1[C:11]([NH:12][CH2:13][C:14]2[CH:23]=[CH:22][C:21]3[C:16](=[CH:17][CH:18]=[CH:19][CH:20]=3)[CH:15]=2)=[CH:10][C:9]([CH2:24][CH3:25])=[C:8]([CH3:26])[N:7]=1)(C)(C)C.Cl.N1C=CC=CC=1>O>[CH2:24]([C:9]1[CH:10]=[C:11]([NH:12][CH2:13][C:14]2[CH:23]=[CH:22][C:21]3[C:16](=[CH:17][CH:18]=[CH:19][CH:20]=3)[CH:15]=2)[C:6](=[S:5])[NH:7][C:8]=1[CH3:26])[CH3:25]

참가 물질

4

반응물 2

HCID 9998883HCID 9998883, 화합물HCID 10176127Pyridinium chloride

생성물 1

HCID 3000382HCID 3000382, 화합물수율 38.4%

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
140 °C

실험 절차

A mixture of 2-tert-butylthio-5-ethyl-6-methyl-3-(2-napthylmethylamino)pyridine (98 mg, 0.27 mmol) and pyridine hydrochloride (0.45 g, 3.8 mmol) was heated under an atmosphere of nitrogen at 140° C. until evolution of gas ceased (about 45 minutes). Water was added and the resultant mixture was extracted three times with chloroform. The organic extracts were combined, dried over anhydrous sodium sulfate, filtered and concentrated under reduced pressure (15 torr). The residue was then subjected to column chromatography on silica gel (eluted with 2% methanol in ethyl acetate). Collection and concentration of appropriate fraction yielded 32 mg (36%) of the pyridinethione. Anal. Calcd for C19H20N2S·0.25 EtOAc: C, 72.68; H, 6.71; N, 8.48. Found: C, 72.41; H, 6.59; N, 8.86.

후처리

  1. custom(about 45 minutes)
  2. extractionthe resultant mixture was extracted three times with chloroform
  3. dry with materialdried over anhydrous sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure (15 torr)
  6. customCollection and concentration of appropriate fraction

출처 및 근거

ORD 기록
ord-e4a453e226234196a081e3b9b0928b78
출처 데이터셋
uspto-grants-1994_05
특허 번호
US05308854

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