N-Methylethylenediamine → HCID 178509325、化合物

HRID 1519754ノート

反応式

HRID 1519754 の反応式
[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

参加物

5

反応物 2

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

生成物 1

HCID 178509325HCID 178509325、化合物収率 99.2%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 25517Ammonium Chloride溶媒

実験手順

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).

後処理

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

出典と根拠

ORDレコード
ord-9aea43d42df04d2f9b8d245d96264029
出典データセット
uspto-grants-2015_07
特許番号
US09073891B2

反応ノート

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