Hydrochloric Acid → 2-Fluoroadenine

HRID 1646671

反応式

HRID 1646671 の反応式
[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

参加物

7

反応物 4

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

生成物 1

HCID 127902-Fluoroadenine収率 52%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 3776Isopropanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-0a9c5e86912d4b8ab8dc6fc81bae9185
出典データセット
uspto-grants-1993_01
特許番号
US05180824

関連ノート

読み込み中…