N-Methylethylenediamine → HCID 178438043, 화합물

HRID 1519829노트

반응식

HRID 1519829 반응식
[Cl:1][C:2]1[C:6]2[C:7]3[N:8]([C:11]([CH2:14][CH3:15])=[N:12][N:13]=3)C=[N:10][C:5]=2[S:4][CH:3]=1.CNCCN>CO.[Cl-].[NH4+]>[Cl:1][C:2]1[C:6]([C:7]2[NH:13][N:12]=[C:11]([CH2:14][CH3:15])[N:8]=2)=[C:5]([NH2:10])[S:4][CH:3]=1

참가 물질

5

반응물 2

HCID 8014N-MethylethylenediamineHCID 687851919-Chloro-3-ethylthieno[3,2-e][1,2,4]triazolo[4,3-c]pyrimidine

생성물 1

HCID 178438043HCID 178438043, 화합물수율 94%

시약·촉매·용매 2

HCID 887Methanol용매HCID 25517Ammonium Chloride용매

실험 절차

9-Chloro-3-ethylthieno[3,2-e][1,2,4]triazolo[4,3-c]pyrimidine (20 mg, 83.8 umol) and N-methylethane-1,2-diamine (0.05 ml, 5.67 umol) in methanol (2 ml) was placed into a preheated oil bath at 60° C. After stirring for 15 min, the solution was diluted with saturated ammonium chloride and extracted with methylene chloride. The combined organic extracts were dried over magnesium sulfate, filtered, and concentrated under reduced pressure to afford 18 mg (94% yield) of 4-chloro-3-(3-ethyl-1H-1,2,4-triazol-5-yl)thiophen-2-amine as a brown solid. Method [8] Retention time 2.63 min by HPLC (M+ 229 and 231).

후처리

  1. extractionextracted with methylene chloride
  2. dry with materialThe combined organic extracts were dried over magnesium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-b85cdb9a13ad435e850b385641caf734
출처 데이터셋
uspto-grants-2015_07
특허 번호
US09073891B2

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