8-Chlorothieno[3,2-e][1,2,4]triazolo[4,3-c]pyrimidine → HCID 178509328、化合物

HRID 1519882ノート

反応式

HRID 1519882 の反応式
[Cl:1][C:2]1[S:10][C:9]2[N:8]=C[N:6]3[CH:11]=[N:12][N:13]=[C:5]3[C:4]=2[CH:3]=1>CO.C(Cl)Cl>[Cl:1][C:2]1[S:10][C:9]([NH2:8])=[C:4]([C:5]2[NH:6][CH:11]=[N:12][N:13]=2)[CH:3]=1

参加物

4

反応物 1

HCID 687834908-Chlorothieno[3,2-e][1,2,4]triazolo[4,3-c]pyrimidine

生成物 1

HCID 178509328HCID 178509328、化合物

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 6344Dichloromethane溶媒

反応条件

温度
60 °C

実験手順

To a stirring mixture of 8-chlorothieno[3,2-e][1,2,4]triazolo[4,3-c]pyrimidine (60 mg, 0.285 mmol) in MeOH (10 mL) was added N-methylethyl 1,2-diamine (106 mg, 1.4 mmol). The resulting mixture was warmed to 60° C. for 1 hr. The reaction mixture was cooled to rt and then diluted with DCM. This mixture was then washed several times with a saturated NH4Cl solution. The organic layer was dried over MgSO4, filtered, and concentrated under reduced pressure to give 5-chloro-3-(4H-1,2,4-triazol-3-yl)thiophen-2-amine. This amine was taken directly to the next coupling reaction without further purification. Retention time (min)=1.227, method [1], MS(ESI) 201.1 (M+H).

後処理

  1. temperatureThe reaction mixture was cooled to rt
  2. washThis mixture was then washed several times with a saturated NH4Cl solution
  3. dry with materialThe organic layer was dried over MgSO4
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-9154884c9712415091267678c44a6f6d
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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