Hydrogen iodide → HCID 178508570, 화합물

HRID 363715노트

반응식

HRID 363715 반응식
Cl[C:2]1[N:10]=[C:9]([NH2:11])[N:8]=[C:7]2[C:3]=1[N:4]=[CH:5][NH:6]2.[IH:12]>O>[I:12][C:2]1[N:10]=[C:9]([NH2:11])[N:8]=[C:7]2[C:3]=1[N:4]=[CH:5][NH:6]2

참가 물질

4

반응물 2

HCID 24841Hydrogen iodideHCID 1785084356-chloro-1H-purin-2-amine

생성물 1

HCID 178508570HCID 178508570, 화합물

시약·촉매·용매 1

HCID 962Water용매

실험 절차

6-Chloro-9H-purin-2-amine (5.0 g., 29.5 mmole) was added to 47% hydrogen iodide (61 ml., 12.2 ml./g.) chilled in an ice bath. After 1.5 hours, water (61 ml.) was added and the mixture stirred in an ice- bath for 30 minutes. The yellow solid was filtered out and the filter cake was washed with water. The wet solid was transferred to a beaker and the residue in the funnel was washed into the beaker with water (30 ml.). 6M Sodium hydroxide (7 ml.) was added with stirring until all the solid had dissolved (pH 14). The solution was added to boiling water (30 ml.) containing acetic acid (3 ml.). The mixture was boiled briefly and allowed to stand at room temperature for one hour. The product was filtered off, washed with water, and dried under vacuum overnight to give 6.88 g. of the desired product; m.p. about 240° C. (dec.).

후처리

  1. temperaturechilled in an ice bath
  2. filtrationThe yellow solid was filtered out
  3. washthe filter cake was washed with water
  4. washthe residue in the funnel was washed into the beaker with water (30 ml.)
  5. addition6M Sodium hydroxide (7 ml.) was added
  6. stirringwith stirring until all the solid
  7. dissolutionhad dissolved (pH 14)
  8. additionThe solution was added
  9. additioncontaining acetic acid (3 ml.)
  10. waitto stand at room temperature for one hour
  11. filtrationThe product was filtered off
  12. washwashed with water
  13. customdried under vacuum overnight
  14. customto give 6.88 g

출처 및 근거

ORD 기록
ord-a665f7367f1844c0ad177ce968f34f39
출처 데이터셋
uspto-grants-1999_02
특허 번호
US05874578

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