HCID 9998883、化合物 → HCID 3000382、化合物

HRID 1033003ノート

反応式

HRID 1033003 の反応式
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]

参加物

4

反応物 2

HCID 9998883HCID 9998883、化合物HCID 10176127Pyridinium chloride

生成物 1

HCID 3000382HCID 3000382、化合物収率 38.4%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
140 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-e4a453e226234196a081e3b9b0928b78
出典データセット
uspto-grants-1994_05
特許番号
US05308854

反応ノート

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