Triethylamine → HCID 178502659, 화합물

HRID 2187235노트

반응식

HRID 2187235 반응식
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]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 11639O-methylhydroxylammonium chlorideHCID 70155832HCID 70155832, 화합물

생성물 1

HCID 178502659HCID 178502659, 화합물수율 31.1%

시약·촉매·용매 1

HCID 6560Isobutanol용매2회

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-8471605050ac46ec9b29b3d11b907ee3
출처 데이터셋
uspto-grants-2002_06
특허 번호
US06407248B1

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