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Potassium Carbonate → 2-[4-[2-(imidazolo[4,5-b]pyridin-2-ylthio)ethyl]piperazin-1-yl]-N-[2,4-bis(methylthio)-6-methyl-3-pyridyl]acetamide

HRID 1064871
ノート
印刷プレビュー

反応式

HRID 1064871 の反応式
[SH:1][C:2]1[NH:3][C:4]2[C:5]([N:10]=1)=[N:6][CH:7]=[CH:8][CH:9]=2.C1OCCOCCOCCOCCOCCOC1.C(=O)([O-])[O-].[K+].[K+].CS(O[CH2:40][CH2:41][N:42]1[CH2:47][CH2:46][N:45]([CH2:48][C:49]([NH:51][C:52]2[C:53]([S:61][CH3:62])=[N:54][C:55]([CH3:60])=[CH:56][C:57]=2[S:58][CH3:59])=[O:50])[CH2:44][CH2:43]1)(=O)=O>CN(C=O)C.O>[NH:3]1[C:4]2[C:5](=[N:6][CH:7]=[CH:8][CH:9]=2)[N:10]=[C:2]1[S:1][CH2:40][CH2:41][N:42]1[CH2:47][CH2:46][N:45]([CH2:48][C:49]([NH:51][C:52]2[C:53]([S:61][CH3:62])=[N:54][C:55]([CH3:60])=[CH:56][C:57]=2[S:58][CH3:59])=[O:50])[CH2:44][CH2:43]1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 11430Potassium CarbonateHCID 2855718-Crown-6HCID 22272586HCID 22272586、化合物HCID 178527819HCID 178527819、化合物

生成物 1

HCID 222727162-[4-[2-(imidazolo[4,5-b]pyridin-2-ylthio)ethyl]piperazin-1-yl]-N-[2,4-bis(methylthio)-6-methyl-3-pyridyl]acetamide収率 40%

試薬・触媒・溶媒 2

HCID 962
Water
溶媒
HCID 6228Dimethylformamide溶媒2 回

実験手順

To a solution of 2-mercaptoimidazolo[4,5-b]pyridine (38.1 mg, 0.252 mmol) in DMF (0.5 ml) were added 18-crown-6 (6.6 mg, 0.025 mmol) and potassium carbonate (63 mg, 0.454 mmol) and the mixture was stirred. Then to the mixture was dropped a solution of crude 2-[4-(2-methanesulfonyloxyethyl)piperazin-1-yl]-N-[2,4-bis(methylthio)-6-methyl-3-pyridyl]acetamide in DMF (1 ml) and stirred at 80° C. for 2 hours. The reaction mixture was diluted with water and extracted with ethyl acetate. The organic layer was washed with water and a saturated sodium chloride solution successively, dried over anhydrous sodium sulfate and concentrated in vacuo. The resulting residue was purified by a silica gel preparative thin layer chromatography (developing solvent; chloroform:methanol=10:1) to provide 51 mg (yield 40%) of the desired compound as colorless powdery crystals. IR (KBr) cm−1: 3140, 1688, 1600, 1564, 1485. 1H-NMR (CDCl3) δ: 2.38 (3H, s), 2.46 (3H, s), 2.49 (3H, s), 2.72-3.00 (10H, m), 3.29 (2H, s), 3.37 (2H, t, J=5.8 Hz), 6.63 (1H, s), 7.12 (1H, dd. J=7.8, 4.9 Hz), 7.82 (1H, d. J=7.8 Hz), 8.25 (1H, d. J=4.9 Hz), 8.49 (1H, br s).

後処理

  1. stirringstirred at 80° C. for 2 hours
  2. extractionextracted with ethyl acetate
  3. washThe organic layer was washed with water
  4. dry with materiala saturated sodium chloride solution successively, dried over anhydrous sodium sulfate
  5. concentrationconcentrated in vacuo
  6. customThe resulting residue was purified by a silica gel preparative thin layer chromatography (developing solvent; chloroform:methanol=10:1)

出典と根拠

ORDレコード
ord-d5fe4e1cbfed47168fb406c3d23e7dfe
出典データセット
uspto-grants-2005_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06969711B2

反応ノート

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