Sulfuric Acid → HCID 178479471, 화합물

HRID 1702608

반응식

HRID 1702608 반응식
[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]

참가 물질

7

반응물 4

HCID 1118Sulfuric AcidHCID 7628Boric AcidHCID 86632-NaphtholHCID 178479474HCID 178479474, 화합물

생성물 1

HCID 178479471HCID 178479471, 화합물

시약·촉매·용매 2

HCID 679Dimethyl Sulfoxide용매HCID 7237O-Xylene용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-86b2ed1f7018499bbbc39add10230690
출처 데이터셋
uspto-grants-1982_09
특허 번호
US04348410

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