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Guanidine → HCID 178468834, 화합물

HRID 1656566
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HRID 1656566 반응식
[NH2:1][C:2]([NH2:4])=[NH:3].[NH2:5][C:6]1O[CH:8]=[C:9]([CH2:13][CH2:14][C:15]2[CH:25]=[CH:24][C:18]([C:19]([O:21][CH2:22][CH3:23])=[O:20])=[CH:17][CH:16]=2)[C:10]=1[C:11]#[N:12]>C(O)C>[NH2:3][C:2]1[NH:4][C:6]2=[N:5][CH:8]=[C:9]([CH2:13][CH2:14][C:15]3[CH:25]=[CH:24][C:18]([C:19]([O:21][CH2:22][CH3:23])=[O:20])=[CH:17][CH:16]=3)[C:10]2=[C:11]([NH2:12])[N:1]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 3520GuanidineHCID 10826899Ethyl 4-[2-(5-amino-4-cyanofuran-3-yl)ethyl]benzoate

생성물 1

HCID 178468834HCID 178468834, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To a solution of guanidine free base (prepared from 105 mg of guanidine hydrochloride and 60 mg of sodium ethoxide) in 10 mL of anhydrous ethanol are added 284 mg (1 mmol) of ethyl 4-[2-(2-amino-3-cyanofur-4-yl)ethyl]benzoate. The mixture is heated at reflux for 30 hrs and the solvent then evaporated in vacuo. The residue is chromatographed on silica gel, eluting with 5:95 methanol:methylene chloride, to yield ethyl 4-{2-(2,4-diaminopyrrolo[2,3-d]pyrimidin-5-yl)ethyl}benzoate as a light brown solid; m.p. 202°-204° C. Mass spectrograph calculated for C17H19N5O2 : 325.1538, Found: 325.1543.

후처리

  1. temperatureThe mixture is heated
  2. temperatureat reflux for 30 hrs
  3. customthe solvent then evaporated in vacuo
  4. customThe residue is chromatographed on silica gel
  5. washeluting with 5:95 methanol

출처 및 근거

ORD 기록
ord-72a670814b5243518c237d3feb9e283a
출처 데이터셋
uspto-grants-1993_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05254687

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