2-Naphthol → HCID 178479471、化合物

HRID 1702607

反応式

HRID 1702607 の反応式
[ClH:1].[NH:2]([CH2:6][C@H:7]1[CH2:12][CH2:11][C@H:10]([C:13]([OH:15])=[O:14])[CH2:9][CH2:8]1)[C:3]([NH2:5])=[NH:4].[CH:16]1[C:25]2[C:20](=[CH:21][CH:22]=[CH:23][CH:24]=2)[CH:19]=[CH:18][C:17]=1O.C1(N=C=NC2CCCCC2)CCCCC1>N1C=CC=CC=1>[ClH:1].[NH:2]([CH2:6][C@H:7]1[CH2:12][CH2:11][C@H:10]([C:13]([O:15][C:18]2[CH:17]=[CH:16][C:25]3[C:20](=[CH:21][CH:22]=[CH:23][CH:24]=3)[CH:19]=2)=[O:14])[CH2:9][CH2:8]1)[C:3]([NH2:5])=[NH:4]

参加物

5

反応物 3

HCID 86632-NaphtholHCID 10868DicyclohexylcarbodiimideHCID 178479474HCID 178479474、化合物

生成物 1

HCID 178479471HCID 178479471、化合物収率 67.9%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

A suspension of trans-4-guanidinomethylcyclohexanecarboxylic acid hydrochloride (47.1 g), β-naphthol (28.8 g) and dicyclohexylcarbodiimide (45.4 g) in pyridine (400 ml) was stirred at room temperature for 24 hours. After evaporation of solvent, to the residue was added water (500 ml), and the mixture was acidified with hydrochloric acid. The resulting white crystals were dissolved in methanol (500 ml). After evaporation of methanol, the residue was recrystallized from methanol to give β-naphtyl trans-4-guanidinomethylcyclohexanecarboxylate hydrochloride (49.1 g, 67.8%), m.p. 195°-202° C.

後処理

  1. customAfter evaporation of solvent
  2. additionto the residue was added water (500 ml)
  3. dissolutionThe resulting white crystals were dissolved in methanol (500 ml)
  4. customAfter evaporation of methanol
  5. customthe residue was recrystallized from methanol

出典と根拠

ORDレコード
ord-f9738bda71e149f6b074ac9ff2555b49
出典データセット
uspto-grants-1982_09
特許番号
US04348410

関連ノート

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