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Cyanamide → HCID 178511002, 화합물

HRID 1253171
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HRID 1253171 반응식
Cl.[NH2:2][C:3]1[CH:7]=[N:6][N:5]([CH2:8][CH2:9][CH2:10][CH2:11][C:12]#[N:13])[N:4]=1.[N:14]#[C:15][NH2:16]>CCO>[NH:2]([C:3]1[CH:7]=[N:6][N:5]([CH2:8][CH2:9][CH2:10][CH2:11][C:12]#[N:13])[N:4]=1)[C:15]([NH2:16])=[NH:14]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 9864Cyanamide2회HCID 20137163HCID 20137163, 화합물

생성물 1

HCID 178511002HCID 178511002, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A solution 5-(4-amino-1,2,3-triazol-2-yl)valeronitrile hydrochloride (2.01 g.) in EtOH (15 ml.) was treated with cyanamide (0.42 g.) and the solution heated under reflux for 4.5 hours. A further 0.1 g. of cyanamide was added and heating under reflux was continued for 2 hours. The solution was evaporated and the residue basified with ammonia and continuously extracted for 24 hours with EtOAc to give a yellow oil which was purified by medium pressure chromatography using chloroform/MeOH/aqueous ammonia (s.g. 0.880) 8:2:0.1 v/v/v as eluant to give 5-(4-guanidino-1,2,3-triazol-2-yl)valeronitrile as a colourless oil (0.45 g.).

후처리

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  1. temperaturethe solution heated
  2. temperatureunder reflux for 4.5 hours
  3. temperatureheating
  4. temperatureunder reflux
  5. customThe solution was evaporated
  6. extractioncontinuously extracted for 24 hours with EtOAc
  7. customto give a yellow oil which
  8. customwas purified by medium pressure chromatography

출처 및 근거

ORD 기록
ord-ba62dbdfb8574d2a820d624b41ad008b
출처 데이터셋
uspto-grants-1988_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04748165

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