N-Methylethylenediamine → HCID 178434595, 화합물

HRID 2098044노트

반응식

HRID 2098044 반응식
[Cl:1][C:2]1[C:6]2[C:7]3[N:8]([C:11]([CH3:14])=[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]([CH3:14])[N:8]=2)=[C:5]([NH2:10])[S:4][CH:3]=1

참가 물질

5

반응물 2

HCID 8014N-MethylethylenediamineHCID 687822379-Chloro-3-methylthieno[3,2-e][1,2,4]triazolo[4,3-c]pyrimidine

생성물 1

HCID 178434595HCID 178434595, 화합물수율 88.1%

시약·촉매·용매 2

HCID 887Methanol용매HCID 25517Ammonium Chloride용매

실험 절차

9-Chloro-3-methylthieno[3,2-e][1,2,4]triazolo[4,3-c]pyrimidine (82 mg, 365 umol) and N-methylethane-1,2-diamine (0.30 ml, 3.40 mmol) 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 69 mg (88% yield) of 4-chloro-3-(3-methyl-1H-1,2,4-triazol-5-yl)thiophen-2-amine as a yellow solid. Method [1] Retention time 0.61 min by HPLC (M+=215 and 217).

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-0c2bdbd770b6466893e9d696d6814828
출처 데이터셋
uspto-grants-2013_05
특허 번호
US08450363B2

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