Hydrochloric Acid → 2-Fluoroadenine

HRID 1646671

반응식

HRID 1646671 반응식
[N:1]([C:4]1[N:12]=[C:11]([F:13])[N:10]=[C:9]2[C:5]=1[NH:6][CH:7]=[N:8]2)=[N+]=[N-].[BH4-].[Na+].Cl.C([O-])([O-])=O.[K+].[K+]>CC(O)C.O>[F:13][C:11]1[N:10]=[C:9]2[C:5]([NH:6][CH:7]=[N:8]2)=[C:4]([NH2:1])[N:12]=1

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 11430Potassium CarbonateHCID 4311764Sodium borohydrideHCID 198012676-azido-2-fluoro-7H-purine

생성물 1

HCID 127902-Fluoroadenine수율 52%

시약·촉매·용매 2

HCID 962Water용매HCID 3776Isopropanol용매

실험 절차

A sample of 6-azido-2-fluoropurine (0.18 g) was dissolved in warm 2-propanol (3 mL) and then cooled to ambient temperature. Sodium borohydride (38 mg) was added in small portions. The vigorous gas evolution was allowed to subside between additions. After the addition was complete the mixture was stirred at ambient temperature and then was heated at 72° C. for 1.5 h. The mixture was then cooled to ambient temperature and diluted with water (10 mL) and the pH was adjusted to 6-7 with 1N hydrochloric acid (HCl) and saturated K2CO3 and then the mixture was concentrated to dryness under vacuum. The residue was triturated in 20 mL of hot water then allowed to cool to ambient temperature. The precipitate was collected by filtration, washed with water and dried to obtain 0.08 g of the title compound as an off-white solid, mp>300° C. This material was identical to an authentic sample by TLC, and IR.

후처리

  1. additionAfter the addition
  2. temperaturewas heated at 72° C. for 1.5 h
  3. temperatureThe mixture was then cooled to ambient temperature
  4. concentrationthe mixture was concentrated to dryness under vacuum
  5. customThe residue was triturated in 20 mL of hot water
  6. temperatureto cool to ambient temperature
  7. filtrationThe precipitate was collected by filtration
  8. washwashed with water
  9. customdried

출처 및 근거

ORD 기록
ord-0a9c5e86912d4b8ab8dc6fc81bae9185
출처 데이터셋
uspto-grants-1993_01
특허 번호
US05180824

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