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Water → HCID 9925691, 화합물

HRID 1602877
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HRID 1602877 반응식
[H-].[Na+].[OH:3][CH2:4][C:5]1[CH:10]=[CH:9][N:8]=[CH:7][CH:6]=1.[CH2:11]([C:15]1[CH:20]=[C:19](Cl)[N:18]2[N:22]=[CH:23][CH:24]=[C:17]2[N:16]=1)[CH2:12][CH:13]=[CH2:14].O>CN(C=O)C>[CH2:11]([C:15]1[CH:20]=[C:19]([O:3][CH2:4][C:5]2[CH:10]=[CH:9][N:8]=[CH:7][CH:6]=2)[N:18]2[N:22]=[CH:23][CH:24]=[C:17]2[N:16]=1)[CH2:12][CH:13]=[CH2:14]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962WaterHCID 114724-HydroxymethylpyridineHCID 24758Sodium hydrideHCID 15462308HCID 15462308, 화합물

생성물 1

HCID 9925691HCID 9925691, 화합물수율 42.7%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

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온도
0 °C

실험 절차

60% sodium hydride, 0.55 g, was added to a 10 ml-solution of 1.6 g of 4-(hydroxymethyl)pyridine in DMF while being ice-cooled. After the mixture was stirred at 0° C. for 30 minutes, a DMF solution (2.5 ml) containing 2.6 g of 5-(3-butenyl)-7-chloropyrazolo[1,5-a]pyrimidine was added dropwise while being ice-cooled. The mixture was stirred at the same temperature for another 1 hour. After completion of the reaction, water was added to the reaction mixture. The crystals precipitated were collected by filtration and washed with water and then with diethyl ether. The crude crystals obtained were recrystallized from ethyl acetate-n-hexane to provide 1.5 g of the title compound as colorless crystals. The structure and melting point of the compound obtained are shown in Table 1.

후처리

  1. temperaturecooled
  2. additionwas added dropwise
  3. temperaturecooled
  4. stirringThe mixture was stirred at the same temperature for another 1 hour
  5. additionwas added to the reaction mixture
  6. customThe crystals precipitated
  7. filtrationwere collected by filtration
  8. washwashed with water
  9. customThe crude crystals obtained
  10. customwere recrystallized from ethyl acetate-n-hexane

출처 및 근거

ORD 기록
ord-4205bc1e009f4dff926864919b0a9bec
출처 데이터셋
uspto-grants-1999_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05985882

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