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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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1-Bromopropane → HCID 13339929, 화합물

HRID 2418682
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HRID 2418682 반응식
[Cl:1][C:2]1[CH:3]=[C:4]2[CH:11]=[N:10][CH:9]([CH3:12])[N:5]2[C:6](=[O:8])[N:7]=1.[H-].[Na+].Br[CH2:16][CH2:17][CH3:18]>O1CCOCC1>[Cl:1][C:2]1[N:7]([CH2:16][CH2:17][CH3:18])[C:6](=[O:8])[N:5]2[C:9]([CH3:12])=[N:10][CH:11]=[C:4]2[CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 78401-BromopropaneHCID 24758Sodium hydrideHCID 70454969HCID 70454969, 화합물

생성물 1

HCID 13339929HCID 13339929, 화합물

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

To a mixture of 2.0 g (10.9 mmole) of 7-chloro-3-methylimidazo[1,5-c]pyrimidin-5-one (from Example 4, Part B) in 50 ml of dioxane was added 0.52 g (13 mmole) of 60% sodium hydride in oil. After ten minutes of stirring, 1.6 g (13 mmole) of 3-bromopropane was added and the mixture was stirred for 16 hours at 50° C. The solution was poured into 100 ml of an ice water mixture. The resulting solution was extracted four times with 75 ml portions of chloroform. The extracts were washed twice with water, dried, and evaporated. The residue was dissolved in 80 ml of chloroform, washed with six 100 ml portions of water, dried and evaporated. The residue was recrystallized with treatment with decolorizing charcoal from cyclohexane to provide 7-chloro-3-methyl-6-n-propylimidazo[1,5-c]pyrimidin-5-one, m.p. 125°-126° C. Analysis: Calculated for C10H12ClNO: %C, 53.2 ; %H, 5.4; %N, 18.6; Found: %C, 53.5; %H, 5.3; %N, 18.6.

후처리

  1. stirringthe mixture was stirred for 16 hours at 50° C
  2. extractionThe resulting solution was extracted four times with 75 ml portions of chloroform
  3. washThe extracts were washed twice with water
  4. customdried
  5. customevaporated
  6. dissolutionThe residue was dissolved in 80 ml of chloroform
  7. washwashed with six 100 ml portions of water
  8. customdried
  9. customevaporated
  10. customThe residue was recrystallized with treatment with decolorizing charcoal from cyclohexane

출처 및 근거

ORD 기록
ord-14af5294041d49db8632775f0a95e610
출처 데이터셋
uspto-grants-1984_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04473570

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