N-Methylethylenediamine → HCID 178509325, 화합물

HRID 1519754노트

반응식

HRID 1519754 반응식
[Br:1][C:2]1[C:6]2[C:7]3[N:8]([CH:11]=[N:12][N:13]=3)C=[N:10][C:5]=2[S:4][CH:3]=1.CNCCN>CO.[Cl-].[NH4+]>[Br:1][C:2]1[C:6]([C:7]2[NH:8][CH:11]=[N:12][N:13]=2)=[C:5]([NH2:10])[S:4][CH:3]=1

참가 물질

5

반응물 2

HCID 8014N-MethylethylenediamineHCID 596366779-Bromothieno[3,2-e][1,2,4]triazolo[4,3-c]pyrimidine

생성물 1

HCID 178509325HCID 178509325, 화합물수율 99.2%

시약·촉매·용매 2

HCID 887Methanol용매HCID 25517Ammonium Chloride용매

실험 절차

9-Bromothieno[3,2-e][1,2,4]triazolo[4,3-c]pyrimidine (551 mg, 2.16 mmol) and N-methylethane-1,2-diamine (1 ml, 11.3 mmol) in methanol (20 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 525 mg (99% yield) of 4-bromo-3-(4H-1,2,4-triazol-3-yl)thiophen-2-amine as a brown solid. Method [8] retention time 2.25 min by HPLC (M+245 and 247).

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-9aea43d42df04d2f9b8d245d96264029
출처 데이터셋
uspto-grants-2015_07
특허 번호
US09073891B2

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