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Hydrochloric Acid → 5-(1'-{[3,5-Diethoxy-4-(1-methyl-1H-pyrazol-4-yl)phenyl]carbonyl}-4-oxospiro[chroman-2,4'-piperidin]-6-yl)pyridine-3-carboxylic acid

HRID 1096898
ノート
印刷プレビュー

反応式

HRID 1096898 の反応式
C(N1C=CN=C1)(N1C=CN=C1)=O.[CH2:13]([O:15][C:16]1[CH:17]=[C:18]([CH:22]=[C:23]([O:31][CH2:32][CH3:33])[C:24]=1[C:25]1[CH:26]=[N:27][N:28]([CH3:30])[CH:29]=1)[C:19](O)=[O:20])[CH3:14].Cl.Cl.[O:36]=[C:37]1[C:51]2[C:46](=[CH:47][CH:48]=[C:49]([C:52]3[CH:53]=[C:54]([C:58]([OH:60])=[O:59])[CH:55]=[N:56][CH:57]=3)[CH:50]=2)[O:45][C:39]2([CH2:44][CH2:43][NH:42][CH2:41][CH2:40]2)[CH2:38]1.Cl>O.C(N(CC)CC)C.CN(C=O)C>[CH2:13]([O:15][C:16]1[CH:17]=[C:18]([C:19]([N:42]2[CH2:41][CH2:40][C:39]3([CH2:38][C:37](=[O:36])[C:51]4[C:46](=[CH:47][CH:48]=[C:49]([C:52]5[CH:53]=[C:54]([C:58]([OH:60])=[O:59])[CH:55]=[N:56][CH:57]=5)[CH:50]=4)[O:45]3)[CH2:44][CH2:43]2)=[O:20])[CH:22]=[C:23]([O:31][CH2:32][CH3:33])[C:24]=1[C:25]1[CH:26]=[N:27][N:28]([CH3:30])[CH:29]=1)[CH3:14]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 313Hydrochloric AcidHCID 682631,1'-CarbonyldiimidazoleHCID 579310273,5-diethoxy-4-(1-methyl-1H-pyrazol-4-yl)benzoic acidHCID 666494905-{4-Oxospiro[chroman-2,4'-piperidin]-6-yl}nicotinic acid di-hydrochloride

生成物 1

HCID 249996275-(1'-{[3,5-Diethoxy-4-(1-methyl-1H-pyrazol-4-yl)phenyl]carbonyl}-4-oxospiro[chroman-2,4'-piperidin]-6-yl)pyridine-3-carboxylic acid

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒2 回HCID 8471Triethylamine溶媒2 回

反応条件

温度
70 °C

実験手順

Carbonyldiimidazole (130 mg) and triethylamine (0.446 mL) were added to a DMF solution (4 mL) of 3,5-diethoxy-4-(1-methyl-1H-pyrazol-4-yl)benzoic acid (232 mg), and stirred at 70° C. for 2 hours. To the reaction liquid, added was a DMF suspension (2 ml) of 5-(4-oxospiro[chroman-2,4′-piperidin]-6-yl)pyridine-3-carboxylic acid dihydrochloride (370 mg) and triethylamine (0.335 ml) that had been prepared separately, and further stirred at that temperature for 1 hour. 1 N hydrochloric acid and water were added to the reaction liquid, the resulting solid was taken out through filtration, and recrystallized from methanol to obtain the title compound.

後処理

  1. customTo the reaction liquid
  2. additionadded
  3. customhad been prepared separately
  4. stirringfurther stirred at that temperature for 1 hour
  5. filtrationthe resulting solid was taken out through filtration
  6. customrecrystallized from methanol

出典と根拠

ORDレコード
ord-e4d71b967deb4ecaa6461ed05cb7bf91
出典データセット
uspto-grants-2012_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08138197B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート