Water → HCID 58196429, 화합물

HRID 2036984노트

반응식

HRID 2036984 반응식
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

참가 물질

5

반응물 3

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

생성물 1

HCID 58196429HCID 58196429, 화합물수율 79%

시약·촉매·용매 1

HCID 13387N-methyl-2-pyrrolidone용매

실험 절차

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]+.

후처리

  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

출처 및 근거

ORD 기록
ord-357b4ebcadb94241b28e27ccdbba1732
출처 데이터셋
uspto-grants-2013_11
특허 번호
US08575177B2

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