Methanol → 1-[2-(6-Methyl-2-pyridyl)ethyl]-4-(4-methylsulfonylaminophenylsulfonyl)piperidine

HRID 373148

反応式

HRID 373148 の反応式
Cl.[CH3:2][S:3]([NH:6][C:7]1[CH:12]=[CH:11][C:10]([S:13]([CH:16]2[CH2:21][CH2:20][NH:19][CH2:18][CH2:17]2)(=[O:15])=[O:14])=[CH:9][CH:8]=1)(=[O:5])=[O:4].[CH3:22][C:23]1[N:28]=[C:27]([CH:29]=[CH2:30])[CH:26]=[CH:25][CH:24]=1.C([O-])(=O)C.[Na+].CO>O>[CH3:22][C:23]1[N:28]=[C:27]([CH2:29][CH2:30][N:19]2[CH2:20][CH2:21][CH:16]([S:13]([C:10]3[CH:11]=[CH:12][C:7]([NH:6][S:3]([CH3:2])(=[O:4])=[O:5])=[CH:8][CH:9]=3)(=[O:15])=[O:14])[CH2:17][CH2:18]2)[CH:26]=[CH:25][CH:24]=1

参加物

6

反応物 4

HCID 887MethanolHCID 707352-Ethenyl-6-methylpyridineHCID 517045Sodium AcetateHCID 185392394-(4-Methylsulfonylaminophenylsulfonyl)piperidine hydrochloride

生成物 1

HCID 150277221-[2-(6-Methyl-2-pyridyl)ethyl]-4-(4-methylsulfonylaminophenylsulfonyl)piperidine収率 64%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

0.60 g (1.86 mmol) of 4-(4-methylsulfonylaminophenylsulfonyl)piperidine hydrochloride obtained in Example 5, 0.44 g (3.72 mmol) of 6-methyl-2-vinylpyridine and 0.31 g of sodium acetate were suspended in 10 ml of a mixture of methanol with water (1:1) and the suspension was refluxed for 2 h. The reaction liquid was filtered and the filtrate was concentrated to give a residue. After extraction with dichloromethane followed by washing with water, the organic layer was concentrated to precipitate white crystals. The crystals were collected by filtration and recrystallized from ethyl acetate to give 0.52 g (yield: 64%) of the intended compound.

後処理

  1. temperaturethe suspension was refluxed for 2 h
  2. customThe reaction liquid
  3. filtrationwas filtered
  4. concentrationthe filtrate was concentrated
  5. customto give a residue
  6. extractionAfter extraction with dichloromethane
  7. washby washing with water
  8. concentrationthe organic layer was concentrated
  9. customto precipitate white crystals
  10. filtrationThe crystals were collected by filtration
  11. customrecrystallized from ethyl acetate

出典と根拠

ORDレコード
ord-e55315fc54894454a029f58dd9684473
出典データセット
uspto-grants-1992_11
特許番号
US05162347

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