Water → HCID 178480023、化合物

HRID 38492ノート

反応式

HRID 38492 の反応式
C1C=CC2N(O)N=NC=2C=1.Cl.[CH3:12][N:13]1[CH:17]=[C:16]([C:18]2[CH:19]=[C:20]3[C:30](=[CH:31][CH:32]=2)[O:29][C:23]2([CH2:28][CH2:27][NH:26][CH2:25][CH2:24]2)[CH2:22][C:21]3=[O:33])[CH:15]=[N:14]1.[CH:34]1([C:37]2[CH:38]=[CH:39][CH:40]=[C:41]3[C:46]=2[N:45]=[C:44]([C:47](O)=[O:48])[CH:43]=[C:42]3[OH:50])[CH2:36][CH2:35]1.O>CN(C=O)C>[CH:34]1([C:37]2[CH:38]=[CH:39][CH:40]=[C:41]3[C:46]=2[N:45]=[C:44]([C:47]([N:26]2[CH2:25][CH2:24][C:23]4([CH2:22][C:21](=[O:33])[C:20]5[C:30](=[CH:31][CH:32]=[C:18]([C:16]6[CH:15]=[N:14][N:13]([CH3:12])[CH:17]=6)[CH:19]=5)[O:29]4)[CH2:28][CH2:27]2)=[O:48])[CH:43]=[C:42]3[OH:50])[CH2:35][CH2:36]1

参加物

6

反応物 4

HCID 962WaterHCID 757711-HydroxybenzotriazoleHCID 667825466-(1-Methyl-1H-pyrazol-4-yl)spiro[chroman-2,4'-piperidin]-4-one hydrochlorideHCID 178524587HCID 178524587、化合物

生成物 1

HCID 178480023HCID 178480023、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide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-(1-methyl-1H-pyrazol-4-yl)spiro[chroman-2,4′-piperidin]-4-one hydrochloride (629 mg, 1.89 mmol) and 8-cyclopropyl-4-hydroxyquinoline-2-carboxylic acid (360 mg, 1.57 mmol) in DMF (3.5 ml) and the mixture was stirred at room temperature overnight. The reaction mixture was poured into water (20 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/AcOEt) to give intended compound as a pale brown 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/AcOEt)
  6. customto give

出典と根拠

ORDレコード
ord-ae09d597526b4d1695d38fdc5e65746c
出典データセット
uspto-grants-2013_09
特許番号
US08524730B2

反応ノート

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