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Water → HCID 57518501, 화합물

HRID 38461
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HRID 38461 반응식
C1C=CC2N(O)N=NC=2C=1.Cl.Cl.[O:13]=[C:14]1[C:28]2[C:23](=[CH:24][CH:25]=[C:26]([C:29]3[CH:37]=[CH:36][C:32]([C:33]([NH2:35])=[O:34])=[CH:31][N:30]=3)[CH:27]=2)[O:22][C:16]2([CH2:21][CH2:20][NH:19][CH2:18][CH2:17]2)[CH2:15]1.[CH2:38]([O:40][C:41]1[CH:46]=[C:45]([C:47](O)=[O:48])[CH:44]=[C:43]([O:50][CH2:51][CH3:52])[C:42]=1[C:53]1[CH:58]=[CH:57][C:56]([C:59]([O:61][CH3:62])=[O:60])=[CH:55][CH:54]=1)[CH3:39].O>CN(C=O)C>[C:33]([C:32]1[CH:36]=[CH:37][C:29]([C:26]2[CH:27]=[C:28]3[C:23](=[CH:24][CH:25]=2)[O:22][C:16]2([CH2:21][CH2:20][N:19]([C:47]([C:45]4[CH:44]=[C:43]([O:50][CH2:51][CH3:52])[C:42]([C:53]5[CH:58]=[CH:57][C:56]([C:59]([O:61][CH3:62])=[O:60])=[CH:55][CH:54]=5)=[C:41]([O:40][CH2:38][CH3:39])[CH:46]=4)=[O:48])[CH2:18][CH2:17]2)[CH2:15][C:14]3=[O:13])=[N:30][CH:31]=1)(=[O:34])[NH2:35]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962WaterHCID 757711-HydroxybenzotriazoleHCID 667818846-(4-Oxospiro[chroman-2,4'-piperidin]-6-yl)nicotinamide dihydrochlorideHCID 670555482,6-Diethoxy-4'-(methoxycarbonyl)biphenyl-4-carboxylic acid

생성물 1

HCID 57518501HCID 57518501, 화합물

시약·촉매·용매 1

HCID 6228
Dimethylformamide
용매

실험 절차

TEA (0.657 ml, 4.71 mmol) was added to a stirred mixture of HOBT (313 mg, 2.04 mmol), WSCDI (361 mg, 1.89 mmol), 6-(4-oxospiro[chroman-2,4′-piperidin]-6-yl)nicotinamide dihydrochloride (2.61 g, 6.97 mmol) and 2,6-diethoxy-4′-(methoxycarbonyl)biphenyl-4-carboxylic acid (2.00 g, 5.81 mmol) in DMF (30 ml) and the mixture was stirred at room temperature for 3 days. The reaction mixture was poured into water (600 ml) and stirred for 30 min. The resulted precipitate was filtered, washed with water and the solid was dried in vacuo at 70° C. The crude product was purified by silicagel column chromatography (CHCl3/Acetone) to give intended compound (3.85 g, quantitative) as a colorless solid.

후처리

  1. stirringstirred for 30 min
  2. filtrationThe resulted precipitate was filtered
  3. washwashed with water
  4. customthe solid was dried in vacuo at 70° C
  5. customThe crude product was purified by silicagel column chromatography (CHCl3/Acetone)
  6. customto give intended compound (3.85 g, quantitative) as a colorless solid

출처 및 근거

ORD 기록
ord-e3c7a1cafabd4e63a22d3aa0c13d5b16
출처 데이터셋
uspto-grants-2013_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08524730B2

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