Triethylamine → HCID 178502659、化合物

HRID 2187235ノート

反応式

HRID 2187235 の反応式
CS[C:3]([NH:8][CH2:9][C:10]1[CH:11]=[N:12][CH:13]=[CH:14][CH:15]=1)=[CH:4][N+:5]([O-:7])=[O:6].[CH3:16][O:17][NH3+:18].[Cl-].C(N(CC)CC)C>C(O)C(C)C>[CH3:16][O:17][N:18]=[C:3]([NH:8][CH2:9][C:10]1[CH:11]=[N:12][CH:13]=[CH:14][CH:15]=1)[CH2:4][N+:5]([O-:7])=[O:6]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 11639O-methylhydroxylammonium chlorideHCID 70155832HCID 70155832、化合物

生成物 1

HCID 178502659HCID 178502659、化合物収率 31.1%

試薬・触媒・溶媒 1

HCID 6560Isobutanol溶媒2 回

実験手順

To 3 ml of isobutyl alcohol was added 0.75 g (0.0033 mole) of 1-methylthio-1-(3-pyridylmethyl)amino-2-nitroethylene, followed by addition of 0.56 g of 0-methylhydroxylamine hydrochloride at 100-110° C. Then, a solution of 0.93 ml of triethylamine in 1 ml of isobutyl alcohol was added dropwise at the same temperature with stirring over a period of 30 minutes. After completion of dropwise addition, the reaction mixture was allowed to cool to room temperature and the solvent was distilled off. The residue was purified by silica gel column chromatography [eluents: MeOH—CHCl3 (1:3) in the first run and MeOH—CHCl3 (1:10) in the second run] to give 0.23 g of the title compound as yellow crystals.

後処理

  1. additionAfter completion of dropwise addition
  2. distillationthe solvent was distilled off
  3. customThe residue was purified by silica gel column chromatography [eluents

出典と根拠

ORDレコード
ord-8471605050ac46ec9b29b3d11b907ee3
出典データセット
uspto-grants-2002_06
特許番号
US06407248B1

反応ノート

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