Sulfuric Acid → HCID 178479471、化合物

HRID 1702608

反応式

HRID 1702608 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.S(=O)(=O)(O)O.B(O)(O)O>CS(C)=O.C1(C)C(C)=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

7

反応物 4

HCID 1118Sulfuric AcidHCID 7628Boric AcidHCID 86632-NaphtholHCID 178479474HCID 178479474、化合物

生成物 1

HCID 178479471HCID 178479471、化合物

試薬・触媒・溶媒 2

HCID 679Dimethyl Sulfoxide溶媒HCID 7237O-Xylene溶媒

実験手順

A suspension of trans-4-guanidinomethylcyclohexanecarboxylic acid hydrochloride(1.8 g), β-naphtol(1.44 g), sulfuric acid(0.05 g) and boric acid(0.03 g) in a mixture of dimethylsulfoxide(10 ml) and xylene(50 ml) was heated under reflux conditions for 20 hours. The resulting water was removed by azeotropy with xylene. Following concentration of the reaction mixture, the residue was chromatographed on a column of silica gel with chloroform/methanol as eluent to give the title compound.

後処理

  1. temperaturewas heated under reflux conditions for 20 hours
  2. customThe resulting water was removed by azeotropy with xylene
  3. customthe residue was chromatographed on a column of silica gel with chloroform/methanol as eluent

出典と根拠

ORDレコード
ord-86b2ed1f7018499bbbc39add10230690
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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