Propylamine → HCID 178446867, 화합물

HRID 892124노트

반응식

HRID 892124 반응식
Cl.[CH2:2]([C@@H:9]1[CH2:20][N:19]2[C:11]([C:12]3[NH:13][C:14]([CH:26]4[CH2:30][CH2:29][CH2:28][CH2:27]4)=[N:15][C:16]=3[N:17]([CH2:22][C:23]([OH:25])=O)[C:18]2=[O:21])=[N:10]1)[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.[CH2:31](N)[CH2:32][CH3:33].Cl.C([N:38]=C=NCCCN(C)C)C>O.O1CCOCC1>[CH2:2]([C@@H:9]1[CH2:20][N:19]2[C:11]([C:12]3[NH:13][C:14]([CH:26]4[CH2:30][CH2:29][CH2:28][CH2:27]4)=[N:15][C:16]=3[N:17]([CH:22]([CH2:31][CH2:32][CH3:33])[C:23]([NH2:38])=[O:25])[C:18]2=[O:21])=[N:10]1)[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1

참가 물질

6

반응물 3

HCID 7852PropylamineHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 178479764HCID 178479764, 화합물

생성물 1

HCID 178446867HCID 178446867, 화합물수율 45.3%

시약·촉매·용매 2

HCID 962Water용매HCID 312751,4-Dioxane용매

실험 절차

Compound 77(50 mg, 0.127 mmol) obtained in Example 77 was dissolved in water (1 mL) and 1,4-dioxane (1 mL), to the solution were added n-propylamine (14 μL, 0.176 mmol, 1.4 equivalents) and 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (24 mg, 0.127 mmol, 1.0 equivalent), and the mixture was stirred at room temperature for 4 days. The reaction solution was extracted with chloroform, and the extract was washed with saturated aqueous sodium chloride, dried over anhydrous magnesium sulfate and concentrated. The residue was purified by silica gel column chromatography (chloroform:methanol=98:2 to 90:10) to obtain the title compound (25 mg, 45%).

후처리

  1. extractionThe reaction solution was extracted with chloroform
  2. washthe extract was washed with saturated aqueous sodium chloride
  3. dry with materialdried over anhydrous magnesium sulfate
  4. concentrationconcentrated
  5. customThe residue was purified by silica gel column chromatography (chloroform:methanol=98:2 to 90:10)

출처 및 근거

ORD 기록
ord-f50ee8462e3d45f49e3848992852fd6d
출처 데이터셋
uspto-grants-2006_02
특허 번호
US07005430B2

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