Triethylamine → HCID 19841185、化合物

HRID 1638784

反応式

HRID 1638784 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][C:12]=1[O:13][CH3:14])[CH:9]=[C:8]([C:15]([OH:17])=O)[CH:7]=[CH:6]2.[ClH:18].Cl.[CH3:20][O:21][C:22]1[CH:23]=[C:24]([CH:32]=[C:33]([O:37][CH3:38])[C:34]=1[O:35][CH3:36])[CH2:25][N:26]1[CH2:31][CH2:30][NH:29][CH2:28][CH2:27]1.C(N(CC)CC)C.P(C#N)(=O)(OCC)OCC>CN(C)C=O>[ClH:18].[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][C:12]=1[O:13][CH3:14])[CH:9]=[C:8]([C:15]([N:29]1[CH2:28][CH2:27][N:26]([CH2:25][C:24]3[CH:32]=[C:33]([O:37][CH3:38])[C:34]([O:35][CH3:36])=[C:22]([O:21][CH3:20])[CH:23]=3)[CH2:31][CH2:30]1)=[O:17])[CH:7]=[CH:6]2

参加物

6

反応物 4

HCID 8471TriethylamineHCID 76257Diethyl cyanophosphonateHCID 2830286,7-Dimethoxy-2-naphthoic acidHCID 128285011-[(3,4,5-Trimethoxyphenyl)methyl]piperazine;dihydrochloride

生成物 1

HCID 19841185HCID 19841185、化合物収率 80.2%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

Using 6,7-dimethoxy-2-naphthoic acid (0.7 g), 1-(3,4,5-trimethoxybenzyl)piperazine dihydrochloride (1.1 g), triethylamine (1.25 g), N,N-dimethylformamide (20 ml) and diethyl phosphorocyanidate (1 ml), an amidation as that described in Example 6 is carried out. The product is purified by silica gel column chromatography (hexane:acetone=2:3) and converted to the hydrochloride in ethyl acetate to give 1-(6,7-dimethoxy-2-naphthoyl)-4-(3,4,5-trimethoxybenzyl)piperazine hydrochloride (1.25 g) as colorless crystals, m.p. 235°-240° C. (decomp.).

後処理

  1. customThe product is purified by silica gel column chromatography (hexane:acetone=2:3)

出典と根拠

ORDレコード
ord-d88993c19b164f389f7cb7893a3868bf
出典データセット
uspto-grants-1989_11
特許番号
US04880809

関連ノート

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