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3,4-Diaminopyridine → HCID 178525444、化合物

HRID 266834
ノート
印刷プレビュー

反応式

HRID 266834 の反応式
[C:1]([CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][O:9][C:10]1[CH:34]=[CH:33][C:13]([C:14]([N:16]2[CH2:21][CH2:20][CH:19]([N:22]3[C:32]4[C:27](=[CH:28][CH:29]=[CH:30][CH:31]=4)[CH2:26][CH2:25][C:23]3=[O:24])[CH2:18][CH2:17]2)=[O:15])=[CH:12][CH:11]=1)([OH:3])=[O:2].[NH2:35][C:36]1[CH:37]=[N:38][CH:39]=[CH:40][C:41]=1[NH2:42].O=P12OP3(OP(OP(O3)(O1)=O)(=O)O2)=O.[CH3:57]S(O)(=O)=O.[OH-].[Na+]>>[NH:42]1[C:41]2[CH:40]=[CH:39][N:38]=[CH:37][C:36]=2[N:35]=[C:57]1[CH:4]([C:1]([OH:3])=[O:2])[CH2:5][CH2:6][CH2:7][CH2:8][O:9][C:10]1[CH:34]=[CH:33][C:13]([C:14]([N:16]2[CH2:17][CH2:18][CH:19]([N:22]3[C:32]4[C:27](=[CH:28][CH:29]=[CH:30][CH:31]=4)[CH2:26][CH2:25][C:23]3=[O:24])[CH2:20][CH2:21]2)=[O:15])=[CH:12][CH:11]=1
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 5

HCID 59183,4-DiaminopyridineHCID 6395Methanesulfonic AcidHCID 14798Sodium HydroxideHCID 14812Phosphorus oxide (P4O10)HCID 190310461-{1-[4-(5-Carboxypentyloxy)benzoyl]-4-piperidinyl}-3,4-dihydrocarbostyril

生成物 1

HCID 178525444HCID 178525444、化合物

実験手順

To 1-{1-[4-(5-carboxypentyloxy)benzoyl]-4-piperidinyl}-3,4-dihydrocarbostyril (2.00 g) are added 3,4-diaminopyridine (0.47 g), phosphorus pentoxide (1.00 g) and methanesulfonic acid (7.0 ml) and the mixture is stirred with heating at 100°-120° C. for 3 hours. After cooling, the reaction solution is poured into ice-water (30 ml) and the mixture is adjusted to around pH 11 with aqueous sodium hydroxide solution and extracted with dichloromethane. The extract is dried with magnesium sulfate and the solvent is distilled off. The resulting residue is purified by silica gel column chromatography (solvent: dichloromethane:methanol=20:1→9:1) to give 1-{1-[4-(5-(imidazo[4,5-c]pyridine-2-yl)carboxypentyloxy)benzoyl]-4-piperidinyl]-3,4-dihydrocarbostyril (1.32 g) as white amorphous form.

後処理

  1. temperaturewith heating at 100°-120° C. for 3 hours
  2. temperatureAfter cooling
  3. extractionextracted with dichloromethane
  4. dry with materialThe extract is dried with magnesium sulfate
  5. distillationthe solvent is distilled off
  6. customThe resulting residue is purified by silica gel column chromatography (solvent: dichloromethane:methanol=20:1→9:1)

出典と根拠

ORDレコード
ord-435a73bbf412487a9679ff0200a53872
出典データセット
uspto-grants-1997_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05652247

反応ノート

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