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Triethylamine → HCID 59853920, 화합물

HRID 2374820
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HRID 2374820 반응식
Cl.C(N=C=NCCCN(C)C)C.[CH3:13][NH:14][CH2:15][CH2:16][CH2:17][CH:18]1[C:28]2[CH:29]=[CH:30][CH:31]=[CH:32][C:27]=2[CH:26]=[CH:25][C:24]2[CH:23]=[CH:22][CH:21]=[CH:20][C:19]1=2.Cl.C(N(CC)CC)C.[C:41]([O:45][C:46]([NH:48][CH2:49][C:50]([OH:52])=O)=[O:47])([CH3:44])([CH3:43])[CH3:42].C(=O)([O-])O.[Na+]>ClCCl>[CH:32]1[C:27]2[CH:26]=[CH:25][C:24]3[CH:23]=[CH:22][CH:21]=[CH:20][C:19]=3[CH:18]([CH2:17][CH2:16][CH2:15][N:14]([CH3:13])[C:50](=[O:52])[CH2:49][NH:48][C:46](=[O:47])[O:45][C:41]([CH3:42])([CH3:43])[CH3:44])[C:28]=2[CH:29]=[CH:30][CH:31]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 5

HCID 8471TriethylamineHCID 78288N-(tert-butoxycarbonyl)glycineHCID 516892Sodium BicarbonateHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 6603149Protriptyline Hydrochloride

생성물 1

HCID 59853920HCID 59853920, 화합물

시약·촉매·용매

1
HCID 6344Dichloromethane용매

실험 절차

134 mg (0.70 mmol) of 1-ethyl-3-(3′-dimethylaminopropyl)carbodiimide hydrochloride, 176 mg (0.59 mmol) of protriptyline hydrochloride and 0.176 ml (1.26 mmol) of triethylamine were added to 129 mg (0.74 mmol) of t-butoxycarbonylglycine in 5 ml of dichloromethane, and they were stirred at room temperature overnight. Saturated aqueous sodium hydrogencarbonate solution was added to the reaction mixture. After extracting with dichloromethane, the organic layer was dried over anhydrous sodium sulfate and then concentrated under reduced pressure. The residue was purified by the silica gel chromatography (hexane:ethyl acetate=3:1) to obtain the title compound.

후처리

  1. extractionAfter extracting with dichloromethane
  2. dry with materialthe organic layer was dried over anhydrous sodium sulfate
  3. concentrationconcentrated under reduced pressure
  4. customThe residue was purified by the silica gel chromatography (hexane:ethyl acetate=3:1)

출처 및 근거

ORD 기록
ord-0e900a9b56b64013b2529e6e0c3f6f6f
출처 데이터셋
uspto-grants-2008_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07462630B2

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