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Water → HCID 57518501、化合物

HRID 38461
ノート
印刷プレビュー

反応式

HRID 38461 の反応式
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]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 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

生成物 1

HCID 57518501HCID 57518501、化合物

試薬・触媒・溶媒 1

HCID 6228
Dimethylformamide
溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-e3c7a1cafabd4e63a22d3aa0c13d5b16
出典データセット
uspto-grants-2013_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08524730B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート