N-Methylethylenediamine → HCID 178434595、化合物

HRID 1519831ノート

反応式

HRID 1519831 の反応式
[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

参加物

5

反応物 2

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

生成物 1

HCID 178434595HCID 178434595、化合物収率 88.1%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 25517Ammonium Chloride溶媒

実験手順

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).

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-98e333faafda4ecf8aad85fea2556d14
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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