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Triethylamine → 5-[[[4-(Dimethylamino)-1-naphthalenyl]carbonyl]amino]-pentanoic acid methyl ester

HRID 1362574
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HRID 1362574 반응식
[CH3:1][N:2]([CH3:16])[C:3]1[C:12]2[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=2)[C:6]([C:13]([OH:15])=O)=[CH:5][CH:4]=1.ON1[C:22](=[O:23])[CH2:21][CH2:20][C:19]1=O.C1(N=C=[N:33][CH:34]2CCCCC2)CCCCC1.C1(/C=C/C=C/[C:50](Cl)=[O:51])C=CC=CC=1.C(N(CC)CC)C>C(Cl)Cl>[CH3:50][O:51][C:22](=[O:23])[CH2:21][CH2:20][CH2:19][CH2:34][NH:33][C:13]([C:6]1[C:7]2[C:12](=[CH:11][CH:10]=[CH:9][CH:8]=2)[C:3]([N:2]([CH3:1])[CH3:16])=[CH:4][CH:5]=1)=[O:15]
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참가 물질

7

반응물 5

HCID 8471TriethylamineHCID 10868DicyclohexylcarbodiimideHCID 80170N-HydroxysuccinimideHCID 5226954-(Dimethylamino)-1-naphthoic acidHCID 6450287(2E,4E)-5-phenylpenta-2,4-dienoyl chloride

생성물 1

HCID 574954285-[[[4-(Dimethylamino)-1-naphthalenyl]carbonyl]amino]-pentanoic acid methyl ester
수율 63%

시약·촉매·용매 1

HCID 6344Dichloromethane용매3회

실험 절차

(Method J9A) To the mixture of 4-(dimethylamino)-1-naphthalenecarboxylic acid (1/62) (0.32 g, 1.5 mmol) and N-hydroxysuccinimide (0.21 g, 1.8 mmol) in methylene chloride (10 ml), dicyclohexylcarbodiimide (0.37 g, 1.8 mmol) in methylene chloride (2 ml) was added. A white precipitate appeared. The reaction mixture was after 0.5 h filtered through a pad of Celite® into the solution of methyl 5-aminopentanoate hydrochloride (2b) (0.33 g, 1.9 mmol) in methylene chloride, followed by the addition of triethylamine (2.6 ml, 19 mmol). The reaction mixture was stirred at room temperature overnight, evaporated, suspended in water and extracted with 3 portions of ethyl acetate. The organic layer was washed with brine and dried (Na2SO4). The solvent was removed and the residue (0.55 g) was purified on silica gel with light petrol-ethyl acetate (2:1) as eluent to give the title compound (0.31 g, 63%), Rf 0.48 (light petrol-ethyl acetate 1:1). 1H NMR (200 MHz, DMSO-d6, TMS) δ: 1.51-1.59 (4H, m), 2.38 (2H, t, 6.9 Hz), 2.85 (6H, s), 3.26-3.36 (m, overlapped with a signal from DMSO), 3.61 (3H, s), 7.08 (1H, d, 7.6 Hz), 7.48-7.57 (3H, m), 8.15-8.27 (2H, m), 8.43 (1H, t, br).

후처리

  1. additionwas added
  2. customevaporated
  3. extractionextracted with 3 portions of ethyl acetate
  4. washThe organic layer was washed with brine
  5. dry with materialdried (Na2SO4)
  6. customThe solvent was removed
  7. customthe residue (0.55 g) was purified on silica gel with light petrol-ethyl acetate (2:1) as eluent

출처 및 근거

ORD 기록
ord-fc1717a97d104caca32e9bb87f9c3b96
출처 데이터셋
uspto-grants-2011_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07880020B2

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