Propylamine → HCID 178446867、化合物

HRID 892124ノート

反応式

HRID 892124 の反応式
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

参加物

6

反応物 3

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

生成物 1

HCID 178446867HCID 178446867、化合物収率 45.3%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 312751,4-Dioxane溶媒

実験手順

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%).

後処理

  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)

出典と根拠

ORDレコード
ord-f50ee8462e3d45f49e3848992852fd6d
出典データセット
uspto-grants-2006_02
特許番号
US07005430B2

反応ノート

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