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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Hydrochloric Acid → HCID 178498876, 화합물

HRID 1285568
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HRID 1285568 반응식
[C:1]([NH:5][CH2:6][CH:7]([OH:24])[CH2:8][O:9][C:10]1[CH:15]=[CH:14][C:13]([C:16]2[NH:17][CH:18]=[C:19]([C:21]([OH:23])=[O:22])[N:20]=2)=[CH:12][CH:11]=1)([CH3:4])([CH3:3])[CH3:2].Cl.[CH3:26]O>>[C:1]([NH:5][CH2:6][CH:7]([OH:24])[CH2:8][O:9][C:10]1[CH:15]=[CH:14][C:13]([C:16]2[NH:17][CH:18]=[C:19]([C:21]([O:23][CH3:26])=[O:22])[N:20]=2)=[CH:12][CH:11]=1)([CH3:4])([CH3:2])[CH3:3]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 313Hydrochloric AcidHCID 887MethanolHCID 178449127HCID 178449127, 화합물

생성물 1

HCID 178498876HCID 178498876, 화합물

실험 절차

A solution of crude 2-[4-(3-tert-butylamino-2-hydroxypropoxy)phenyl]-4-carboxyimidazole ◯1 (30 g.) in methanol (600 ml.) is heated to reflux, and then heating is discontinued as hydrogen chloride is bubbled rapidly through the solution with stirring for a half hour, followed by two and a half hours at reflux. Bubbling of hydrogen chloride is continued for another two hours followed by another hour at reflux and then the reaction mixture is stirred at room temperature overnight. The mixture is filtered and the filtrate is then concentrated to dryness under reduced pressure. The residue is dissolved in water (150 ml.) and the pH is adjusted to 8 with saturated sodium carbonate solution. The basic mixture is extracted with ethyl acetate and the extracts are dried, filtered, and concentrated under reduced pressure to yield a solid which is recrystallized from acetonitrile to yield the methyl 2-[4-(3-tert.butylamino-2-hydroxypropoxy)phenyl]-imidazole-4-carboxylate as a cream-colored solid, m.p. 168°-172° C.

후처리

  1. temperatureto reflux
  2. temperatureheating
  3. customis bubbled rapidly through the solution
  4. waitfollowed by two and a half hours
  5. temperatureat reflux
  6. customBubbling of hydrogen chloride
  7. waitfollowed by another hour
  8. temperatureat reflux
  9. stirringthe reaction mixture is stirred at room temperature overnight
  10. filtrationThe mixture is filtered
  11. concentrationthe filtrate is then concentrated to dryness under reduced pressure
  12. dissolutionThe residue is dissolved in water (150 ml.)
  13. extractionThe basic mixture is extracted with ethyl acetate
  14. customthe extracts are dried
  15. filtrationfiltered
  16. concentrationconcentrated under reduced pressure
  17. customto yield a solid which
  18. customis recrystallized from acetonitrile

출처 및 근거

ORD 기록
ord-8e078dd2119b470ebe950132ab159a1e
출처 데이터셋
uspto-grants-1986_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04567276

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