Water → HCID 19608363, 화합물

HRID 1602879노트

반응식

HRID 1602879 반응식
[CH2:1]([C:5]1[CH:10]=[C:9]([O:11][CH2:12][C:13]2[CH:18]=[CH:17][N:16]=[CH:15][CH:14]=2)[N:8]2[N:19]=[CH:20][CH:21]=[C:7]2[N:6]=1)[CH2:2][CH:3]=[CH2:4].C1C(=O)N([Br:29])C(=O)C1.O>C(COC)OC.O>[Br:29][C:21]1[CH:20]=[N:19][N:8]2[C:9]([O:11][CH2:12][C:13]3[CH:18]=[CH:17][N:16]=[CH:15][CH:14]=3)=[CH:10][C:5]([CH2:1][CH2:2][CH:3]=[CH2:4])=[N:6][C:7]=12

참가 물질

5

반응물 3

HCID 962WaterHCID 67184N-bromobutanimideHCID 9925691HCID 9925691, 화합물2회

생성물 1

HCID 19608363HCID 19608363, 화합물

시약·촉매·용매 1

HCID 18180031Water 1,2-dimethoxyethane용매

반응 조건

온도
0 °C

실험 절차

5-(3-Butenyl)-7-(4-pyridylmethoxy)pyrazolo[1,5-a]pyrimidine (compound of Example 1), 500 mg, was dissolved in 10 ml of dimethoxyethane-water (3:1). The solution was cooled to 0° C. and 380 mg of NBS was added. The mixture was stirred at 0° C. for 1 hour and further stirred at room temperature for 1 hour. Water was added to the reaction mixture and the crystals precipitated were collected by filtration. The crude crystals were recrystallized from dichloromethane-n-hexane to provide 440 mg of the title compound as colorless crystals. The structure and melting point of the compound obtained are shown in Table 1.

후처리

  1. stirringfurther stirred at room temperature for 1 hour
  2. customthe crystals precipitated
  3. filtrationwere collected by filtration
  4. customThe crude crystals were recrystallized from dichloromethane-n-hexane

출처 및 근거

ORD 기록
ord-29521f189ae341d2855afa7aeb173097
출처 데이터셋
uspto-grants-1999_11
특허 번호
US05985882

반응 노트

불러오는 중…