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Triethylamine → Hexyl 2-[[[4-[[4-[(dipropylamino)methyl]phenyl]carbamoyl]phenyl]methyl-[(1-hexoxycarbonylimidazol-2-yl)methyl]amino]methyl]imidazole-1-carboxylate

HRID 1173948
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HRID 1173948 반응식
[NH:1]1[CH:5]=[CH:4][N:3]=[C:2]1[CH2:6][N:7]([CH2:14][C:15]1[CH:37]=[CH:36][C:18]([C:19]([NH:21][C:22]2[CH:27]=[CH:26][C:25]([CH2:28][N:29]([CH2:33][CH2:34][CH3:35])[CH2:30][CH2:31][CH3:32])=[CH:24][CH:23]=2)=[O:20])=[CH:17][CH:16]=1)[CH2:8][C:9]1[NH:10][CH:11]=[CH:12][N:13]=1.Cl[C:39]([O:41][CH2:42][CH2:43][CH2:44][CH2:45][CH2:46][CH3:47])=[O:40].C(N([CH2:53][CH3:54])CC)C>C(Cl)(Cl)Cl>[CH2:42]([O:41][C:39]([N:1]1[CH:5]=[CH:4][N:3]=[C:2]1[CH2:6][N:7]([CH2:14][C:15]1[CH:37]=[CH:36][C:18]([C:19]([NH:21][C:22]2[CH:23]=[CH:24][C:25]([CH2:28][N:29]([CH2:33][CH2:34][CH3:35])[CH2:30][CH2:31][CH3:32])=[CH:26][CH:27]=2)=[O:20])=[CH:17][CH:16]=1)[CH2:8][C:9]1[N:13]([C:39]([O:41][CH2:42][CH2:43][CH2:44][CH2:45][CH2:53][CH3:54])=[O:40])[CH:12]=[CH:11][N:10]=1)=[O:40])[CH2:43][CH2:44][CH2:45][CH2:46][CH3:47]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 22466Hexyl chloroformateHCID 99834204-{[bis(1H-imidazol-2-ylmethyl)-amino]-methyl}-N-(4-dipropylaminomethylphenyl)-benzamide

생성물 1

HCID 58801928Hexyl 2-[[[4-[[4-[(dipropylamino)methyl]phenyl]carbamoyl]phenyl]methyl-[(1-hexoxycarbonylimidazol-2-yl)methyl]amino]methyl]imidazole-1-carboxylate

시약·촉매·용매 1

HCID 6212
Chloroform
용매

실험 절차

The compound obtained in Example 19-3 was treated with an anion-exchange resin. The treated product was dissolved in chloroform (4.0 ml) and added with n-hexyl chloroformate (manufactured by Tokyo Kasei Kogyo Co., Ltd.) (0.054 ml) and triethylamine (0.060 ml), followed by stirring at room temperature for 16 hours. After completion of the reaction, the solvent was distilled off. The residue was added with chloroform, washed with water and saturated saline solution, and dried with anhydrous sodium sulfate, followed by distilling the solvent off. Subsequently, the residue was purified through silica gel column chromatography (chloroform/methanol), thereby obtaining the subject compound (66.6 mg) as a white solid.

후처리

  1. customAfter completion of the reaction
  2. distillationthe solvent was distilled off
  3. additionThe residue was added with chloroform
  4. washwashed with water and saturated saline solution
  5. dry with materialdried with anhydrous sodium sulfate
  6. distillationby distilling the solvent off
  7. customSubsequently, the residue was purified through silica gel column chromatography (chloroform/methanol)

출처 및 근거

ORD 기록
ord-d59d26ac3c6041bd93e3301c512ec756
출처 데이터셋
uspto-grants-2010_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07833991B2

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