Water → HCID 58196429、化合物

HRID 2036984ノート

反応式

HRID 2036984 の反応式
Cl[C:2]1[N:7]2[N:8]=[CH:9][CH:10]=[C:6]2[N:5]=[C:4]([S:11][CH3:12])[N:3]=1.[CH:13]1([NH2:16])[CH2:15][CH2:14]1.O>CN1C(=O)CCC1>[CH:13]1([NH:16][C:2]2[N:7]3[N:8]=[CH:9][CH:10]=[C:6]3[N:5]=[C:4]([S:11][CH3:12])[N:3]=2)[CH2:15][CH2:14]1

参加物

5

反応物 3

HCID 962WaterHCID 69828CyclopropylamineHCID 129161154-Chloro-2-(methylthio)pyrazolo[1,5-a][1,3,5]triazine

生成物 1

HCID 58196429HCID 58196429、化合物収率 79%

試薬・触媒・溶媒 1

HCID 13387N-methyl-2-pyrrolidone溶媒

実験手順

4-Chloro-2-(methylthio)pyrazolo[1,5-a][1,3,5]triazine (1.0 eq, 6.26 g, 31.19 mmol) was suspended in anhydrous NMP (50 ml). Cyclopropylamine (1.5 eq, 3.2 ml, 46.26 mmol) was added through syringe dropwise. Internal temperature rose to 47° C. The mixture was stirred without any external cooling for one hour. An additional amount of cypropylamine (1 ml) was added and the mixture stirred for another 1.5 hours. The mixture was slowly poured into water (500 ml) under stirring. The resulting solid was filtered, washed with water and dried in a vacuum oven to give N-cyclopropyl-2-(methylthio)pyrazolo[1,5-a][1,3,5]triazin-4-amine as a tan solid (5.44 g, 79% yield). LCMS (ES):>95% pure, m/z 222 [M+H]+.

後処理

  1. customrose to 47° C
  2. temperatureany external cooling for one hour
  3. additionAn additional amount of cypropylamine (1 ml) was added
  4. stirringthe mixture stirred for another 1.5 hours
  5. stirringunder stirring
  6. filtrationThe resulting solid was filtered
  7. washwashed with water
  8. customdried in a vacuum oven

出典と根拠

ORDレコード
ord-357b4ebcadb94241b28e27ccdbba1732
出典データセット
uspto-grants-2013_11
特許番号
US08575177B2

反応ノート

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