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4-Benzylpiperazine-1-carboxamidine hemisulfate → HCID 178520340, 화합물

HRID 1032697
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HRID 1032697 반응식
[Na].[OH:2][CH:3]=[C:4]1[CH2:9][CH2:8][O:7][C:5]1=O.S(O)(O)(=O)=O.[C:15]([N:18]1[CH2:23][CH2:22][N:21]([CH2:24][C:25]2[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=2)[CH2:20][CH2:19]1)(=[NH:17])[NH2:16]>C(O)C>[CH2:24]([N:21]1[CH2:20][CH2:19][N:18]([C:15]2[N:17]=[C:3]([OH:2])[C:4]([CH2:9][CH2:8][OH:7])=[CH:5][N:16]=2)[CH2:23][CH2:22]1)[C:25]1[CH:26]=[CH:27][CH:28]=[CH:29][CH:30]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 27566524-Benzylpiperazine-1-carboxamidine hemisulfateHCID 66988753HCID 66988753, 화합물

생성물 1

HCID 178520340HCID 178520340, 화합물수율 29%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

10.0 g (73.5 mmoles) of 2-hydroxymethylenebutyrolactone sodium salt [synthesized by the method described in J. O. Fissekis et al., J. Org., Chem. 29, 2670 (1964)] and 19.6 g (73.3 mmoles) of 1-amidino-4-benzylpiperazine sulfate were added to 360 ml of ethanol, and the solution was refluxed for 5 hours. Ethanol was evaporated, and the residue was mixed with water and extracted with chloroform. The chloroform layer was dried, concentrated, and purified by silica gel column chromatography to give 6.66 g (yield 29%) of 2-(4-benzylpiperazino)-4-hydroxy-5-(2-hydroxyethyl)pyrimidine as crystals.

후처리

  1. temperaturethe solution was refluxed for 5 hours
  2. customEthanol was evaporated
  3. additionthe residue was mixed with water
  4. extractionextracted with chloroform
  5. dry with materialThe chloroform layer was dried
  6. concentrationconcentrated
  7. custompurified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-dd64aadefc88404db465c46502ead374
출처 데이터셋
uspto-grants-1990_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04959368

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