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Ammonia → HCID 13569205, 화합물

HRID 980145
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HRID 980145 반응식
P(Cl)(Cl)(Cl)(Cl)Cl.Cl[S:8]([OH:11])(=O)=[O:9].[O:12]([CH2:19][CH2:20][N:21]1[CH:25]=[CH:24][N:23]=[CH:22]1)[C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1.[NH3:26]>>[S:8]([C:16]1[CH:17]=[CH:18][C:13]([O:12][CH2:19][CH2:20][N:21]2[CH:25]=[CH:24][N:23]=[CH:22]2)=[CH:14][CH:15]=1)(=[O:11])(=[O:9])[NH2:26]
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5

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HCID 222AmmoniaHCID 24638Chlorosulfonic acidHCID 24819Phosphorus pentachlorideHCID 135691721H-Imidazole, 1-(2-phenoxyethyl)-

생성물 1

HCID 13569205HCID 13569205, 화합물

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온도
0 °C

실험 절차

Phosphorus pentachloride (2.08 g) was added cautiously to chlorosulphonic acid (2.91 g) and the resulting solution was cooled to 0° C. 1-(2-Phenoxyethyl)imidazole (1.88 g) was added in portions, allowing the effervescence to subside after each addition. The mixture was heated on a steam bath for 10 minutes, cooled, and poured onto a mixture of crushed ice and excess concentrated ammonia solution. The resulting gummy solid was filtered off, washed with water, sucked as dry as possible at the filter pump and chromatographed on silica gel. Elution with a mixture of chloroform and methanol (4:1) gave a gum which crystallised on trituration with a few mls. of ethanol. The solid was crystallised from ethanol to give 1-[2-(4-sulphamoylphenoxy)ethyl]imidazole (0.5 g), m.p. 147.5°-148.5° C. Found: C, 49.57; H, 4.93; N, 15.36. C11H13N3O3S requires: C, 49.42; H, 4.90; N, 15.72%.

후처리

  1. additionafter each addition
  2. temperatureThe mixture was heated on a steam bath for 10 minutes
  3. temperaturecooled
  4. filtrationThe resulting gummy solid was filtered off
  5. washwashed with water
  6. customas dry as possible at the filter pump
  7. customchromatographed on silica gel
  8. washElution
  9. additionwith a mixture of chloroform and methanol (4:1)
  10. customgave a gum which
  11. customcrystallised on trituration with a few mls
  12. customThe solid was crystallised from ethanol

출처 및 근거

ORD 기록
ord-d4ffb15526a74adeb545a2b1c9fb893d
출처 데이터셋
uspto-grants-1987_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04636500

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