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1-(2-Hydroxyethyl)piperazine → 2-(4'-beta-Hydroxyethyl-piperazino)-5-oxo-6-carbethoxy-8-ethylpyrido(2,3-d)pyrimidine

HRID 66000
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HRID 66000 반응식
Cl[C:2]1[N:3]=[CH:4][C:5]2[C:11](=[O:12])[C:10]([C:13]([O:15][CH2:16][CH3:17])=[O:14])=[CH:9][N:8]([CH2:18][CH3:19])[C:6]=2[N:7]=1.[OH:20][CH2:21][CH2:22][N:23]1[CH2:28][CH2:27][NH:26][CH2:25][CH2:24]1>C1(C)C=CC=CC=1>[OH:20][CH2:21][CH2:22][N:23]1[CH2:28][CH2:27][N:26]([C:2]2[N:3]=[CH:4][C:5]3[C:11](=[O:12])[C:10]([C:13]([O:15][CH2:16][CH3:17])=[O:14])=[CH:9][N:8]([CH2:18][CH3:19])[C:6]=3[N:7]=2)[CH2:25][CH2:24]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 76771-(2-Hydroxyethyl)piperazineHCID 122668052-Chloro-5-oxo-6-carbethoxy-8-ethyl-5,8-dihydropyrido(2,3-d)pyrimidine

생성물 1

HCID 227568342-(4'-beta-Hydroxyethyl-piperazino)-5-oxo-6-carbethoxy-8-ethylpyrido(2,3-d)pyrimidine수율 68%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

5.6 g. of 2-chloro-5-oxo-6-carbethoxy-8-ethyl-5,8-dihydro-pyrido(2,3-d)pyrimidine, 5.2 g. of 1-β-hydroxyethyl piperazine and 50 cm3 of toluene are heated under reflux for 2 hours. After cooling, the solution is filtered to remove the hydrochloride which has precipitated, and the organic solution is diluted with its own volume of chloroform, is washed with water and dried (MgSO4). After evaporation, the residue is recrystallised from 40 cm3 of a mixture of isopropanol (1 volume) and isopropyl ether (2 volumes). 5.14 g. (68%) of 2-(4'-β-hydroxyethyl-piperazino)-5-oxo-6-carbethoxy-8-ethylpyrido(2,3-d)pyrimidine are obtained; melting point 172° C.

후처리

  1. temperatureunder reflux for 2 hours
  2. temperatureAfter cooling
  3. filtrationthe solution is filtered
  4. customto remove the hydrochloride which
  5. customhas precipitated
  6. additionthe organic solution is diluted with its own volume of chloroform
  7. washis washed with water
  8. dry with materialdried (MgSO4)
  9. customAfter evaporation
  10. customthe residue is recrystallised from 40 cm3 of a mixture of isopropanol (1 volume) and isopropyl ether (2 volumes)

출처 및 근거

ORD 기록
ord-f9a24339bd324d649a5bc310dd06507a
출처 데이터셋
uspto-grants-1978_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04129737

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