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Triethylamine → HCID 18918517, 화합물

HRID 864782
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HRID 864782 반응식
Cl.Cl.[N:3]1[CH:8]=[CH:7][C:6]([N:9]2[CH2:14][CH2:13][N:12]([CH2:15][C:16]([OH:18])=O)[CH2:11][CH2:10]2)=[CH:5][CH:4]=1.[CH2:19](N(CC)CC)[CH3:20].C1C=CC2N(O)N=NC=2C=1.C(N=C=NC(C)C)(C)C.C([N:47]1[CH2:52][CH2:51][CH:50]([CH2:53][C:54]([OH:56])=[O:55])[CH2:49][CH2:48]1)C>CN(C)C=O>[N:3]1[CH:4]=[CH:5][C:6]([N:9]2[CH2:10][CH2:11][N:12]([CH2:15][C:16]([N:47]3[CH2:48][CH2:49][CH:50]([CH2:53][C:54]([O:56][CH2:19][CH3:20])=[O:55])[CH2:51][CH2:52]3)=[O:18])[CH2:13][CH2:14]2)=[CH:7][CH:8]=1
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7

반응물 5

HCID 8471TriethylamineHCID 12734DiisopropylcarbodiimideHCID 757711-HydroxybenzotriazoleHCID 18918276(1-Ethylpiperidin-4-yl)acetic acidHCID 189185271-Piperazineacetic acid, 4-(4-pyridinyl)-, hydrochloride (1:2)

생성물 1

HCID 18918517HCID 18918517, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A solution containing 1-(4-pyridyl)-4-carboxymethylpiperazine dihydrochloride 1/4H2O(400 mg, 1.33 mMoles), triethylamine (0.4 ml, 2.66 mMoles) and HOBT (0.2 g, 1.46 mMoles) in dry dimethylformamide (20 ml) was treated with diisopropylcarbodiimide (0.23 ml, 1.46 mMoles) and the mixture was stirred for 5 minutes. Ethyl 4-carboxymethylpiperidine was added and the mixture was stirred for a further 4 hours. The mixture was concentrated to half volume under reduced pressure and then poured into water (50 ml) and extracted with ethyl acetate (3×20 ml) and dichloromethane (3×20 ml). The combined organic extracts were concentrated under reduced pressure and the residue was purified by chromatography (flash column made with grade III alumina and eluted with a gradient of 0-1% methanol in dichloromethane) to give the title compound (130 mg) as a colourless oil; NMR (d6DMSO): 0.9-1.1 (m,2H), 1.2 (t,3H), 1.65 (d,2H), 1.8-2.0 (m,1H), 2.2 (d,2H), 2.5 (m,2H), 2.9-3.4 (m,10H), 4.0 (q,2H+m,1H), 4.3 (d,1H), 6.8 (d,2H), 8.15 (d,2H); m/e 375 (M+H)+.

후처리

  1. stirringthe mixture was stirred for a further 4 hours
  2. concentrationThe mixture was concentrated to half volume under reduced pressure
  3. additionpoured into water (50 ml)
  4. extractionextracted with ethyl acetate (3×20 ml) and dichloromethane (3×20 ml)
  5. concentrationThe combined organic extracts were concentrated under reduced pressure
  6. customthe residue was purified by chromatography (flash column
  7. washeluted with a gradient of 0-1% methanol in dichloromethane)

출처 및 근거

ORD 기록
ord-73cb8c9fe4dc46848a69624c10747b1e
출처 데이터셋
uspto-grants-1996_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05563141

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