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1,4-Dioxane hydrochloride → HCID 67103529, 화합물

HRID 2080770
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HRID 2080770 반응식
[CH3:1][O:2][C:3](=[O:29])[C:4]1[CH:9]=[CH:8][C:7]([NH2:10])=[C:6]([N:11]([C:13](=O)[C:14]2[CH:19]=[CH:18][CH:17]=[C:16]([CH2:20][N:21]([CH2:25][CH2:26][CH3:27])[CH2:22][CH2:23][CH3:24])[CH:15]=2)[CH3:12])[CH:5]=1.Cl.O1CCOCC1>CO>[CH3:1][O:2][C:3]([C:4]1[CH:9]=[CH:8][C:7]2[N:10]=[C:13]([C:14]3[CH:19]=[CH:18][CH:17]=[C:16]([CH2:20][N:21]([CH2:25][CH2:26][CH3:27])[CH2:22][CH2:23][CH3:24])[CH:15]=3)[N:11]([CH3:12])[C:6]=2[CH:5]=1)=[O:29]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 204431481,4-Dioxane hydrochlorideHCID 671037494-Amino-3-[(3-dipropylaminomethyl-benzoyl)-methyl-amino]-benzoic acid methyl ester

생성물 1

HCID 67103529HCID 67103529, 화합물수율 55.5%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

The compound (83.0 mg) obtained in Example 18-4 was dissolved in methanol (1.0 ml) and added with a 4 mol/l hydrogen chloride/dioxane solution (1.0 ml) and the whole was stirred at room temperature for 6 hours. After completion of the reaction, the solvent was distilled off under reduced pressure. The residue was dissolved in methanol to generate a free compound therefrom through an anion-exchange resin (Amberlite IRA-410). The resin was separated by filtration and the filtrate subjected to distillation of the solvent under reduced pressure. The residue was purified through silica gel column chromatography (chloroform/ethyl acetate), thereby obtaining the subject compound (44.0 mg) as a brown solid.

후처리

  1. customAfter completion of the reaction
  2. distillationthe solvent was distilled off under reduced pressure
  3. dissolutionThe residue was dissolved in methanol
  4. customThe resin was separated by filtration
  5. distillationthe filtrate subjected to distillation of the solvent under reduced pressure
  6. customThe residue was purified through silica gel column chromatography (chloroform/ethyl acetate)

출처 및 근거

ORD 기록
ord-2dc1b11aab784de9a86f7481f16d11c8
출처 데이터셋
uspto-grants-2011_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07932281B2

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