Triethylamine → 1-(6,7-Dibutoxy-2-naphthoyl)-4-(3,4,5-trimethoxybenzyl)piperazine hydrochloride

HRID 1638785ノート

反応式

HRID 1638785 の反応式
[CH2:1]([O:5][C:6]1[CH:7]=[C:8]2[C:13](=[CH:14][C:15]=1[O:16][CH2:17][CH2:18][CH2:19][CH3:20])[CH:12]=[C:11]([C:21]([OH:23])=O)[CH:10]=[CH:9]2)[CH2:2][CH2:3][CH3:4].[ClH:24].Cl.[CH3:26][O:27][C:28]1[CH:29]=[C:30]([CH:38]=[C:39]([O:43][CH3:44])[C:40]=1[O:41][CH3:42])[CH2:31][N:32]1[CH2:37][CH2:36][NH:35][CH2:34][CH2:33]1.C(N(CC)CC)C.P(C#N)(=O)(OCC)OCC>CN(C)C=O>[ClH:24].[CH2:1]([O:5][C:6]1[CH:7]=[C:8]2[C:13](=[CH:14][C:15]=1[O:16][CH2:17][CH2:18][CH2:19][CH3:20])[CH:12]=[C:11]([C:21]([N:35]1[CH2:34][CH2:33][N:32]([CH2:31][C:30]3[CH:38]=[C:39]([O:43][CH3:44])[C:40]([O:41][CH3:42])=[C:28]([O:27][CH3:26])[CH:29]=3)[CH2:37][CH2:36]1)=[O:23])[CH:10]=[CH:9]2)[CH2:2][CH2:3][CH3:4]

参加物

6

反応物 4

HCID 8471TriethylamineHCID 76257Diethyl cyanophosphonateHCID 128285011-[(3,4,5-Trimethoxyphenyl)methyl]piperazine;dihydrochlorideHCID 146761936,7-Dibutoxy-2-naphthoic acid

生成物 1

HCID 198412421-(6,7-Dibutoxy-2-naphthoyl)-4-(3,4,5-trimethoxybenzyl)piperazine hydrochloride収率 84.2%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

Using 6,7-dibutoxy-2-naphthoic acid (0.25 g), 1-(3,4,5-trimethoxybenzyl)piperazine dihydrochloride (0.31 g), triethylamine (0.35 g), N,N-dimethylformamide (10 ml) and diethyl phosphorocyanidate (0.5 ml), an amidation as that described in Example 6 is carried out. The reaction mixture is purified by gel column chromatography (hexane:acetone=1:1) and converted to the hydrochloride in ethyl acetate to give 1-(6,7-dibutoxy-2-naphthoyl)-4-(3,4,5-trimethoxybenzyl)piperazine hydrochloride (0.4 g) as colorless prisms, m.p. 182°-185° C.

後処理

  1. customThe reaction mixture is purified by gel column chromatography (hexane:acetone=1:1)

出典と根拠

ORDレコード
ord-10f32baff4434981a2195c42437e77cb
出典データセット
uspto-grants-1989_11
特許番号
US04880809

反応ノート

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