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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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HCID 3042017, 화합물 → HCID 18919350, 화합물

HRID 1290815
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HRID 1290815 반응식
[Cl:1][CH:2]=[CH:3][C:4](=O)[CH2:5]Cl.ClC=CC(=O)C(C)C.[NH2:16][C:17]1[N:21]=[CH:20][NH:19][N:18]=1>C(O)(=O)C>[Cl:1][CH2:2][C:3]1[N:18]2[N:19]=[CH:20][N:21]=[C:17]2[N:16]=[CH:5][CH:4]=1
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HCID 3042017HCID 3042017, 화합물HCID 53421801HCID 53421801, 화합물HCID 178418311HCID 178418311, 화합물

생성물 1

HCID 18919350HCID 18919350, 화합물

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

1,4-Dichloro-1-buten-3-one (10.9 g) (prepared in a manner analogous to the preparation of 1-chloro-4-methyl-1-penten-3-one described in Example 20 below), 3-amino-1,2,4-triazole (6.5 g) and glacial acetic acid were heated under reflux for 1 hour and 30 minutes. The reaction mixture was poured onto ice and extracted with dichloromethane. The organic layer was dried over magnesium sulphate and the solvent was evaporated to give a solid. The crude product was purified by flash chromatography using as eluent a mixture of dichloromethane and ethanol (in the ratio 97:3 respectively), followed by recrystallisation from tetrachloromethane, to give 7-chloromethyl-1,2,4-triazolo[1,5-a]pyrimidine. Yield 10.15 g.

후처리

  1. temperaturewere heated
  2. temperatureunder reflux for 1 hour and 30 minutes
  3. additionThe reaction mixture was poured onto ice
  4. extractionextracted with dichloromethane
  5. dry with materialThe organic layer was dried over magnesium sulphate
  6. customthe solvent was evaporated
  7. customto give a solid
  8. customThe crude product was purified by flash chromatography
  9. additiona mixture of dichloromethane and ethanol (in the ratio 97:3 respectively),
  10. customfollowed by recrystallisation from tetrachloromethane

출처 및 근거

ORD 기록
ord-026c8a65562c4e2b93e9ac28749e2220
출처 데이터셋
uspto-grants-1998_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05753665

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