4-Fluorobenzyl chloride → 6-Amino-2-chloro-9-(4-fluorobenzyl)purine

HRID 2269146

반응식

HRID 2269146 반응식
[NH2:1][C:2]1[N:10]=[C:9]([Cl:11])[N:8]=[C:7]2[C:3]=1[NH:4][CH:5]=[N:6]2.C(=O)([O-])[O-].[K+].[K+].[F:18][C:19]1[CH:26]=[CH:25][C:22]([CH2:23]Cl)=[CH:21][CH:20]=1>CN(C=O)C>[NH2:1][C:2]1[N:10]=[C:9]([Cl:11])[N:8]=[C:7]2[C:3]=1[N:4]=[CH:5][N:6]2[CH2:23][C:22]1[CH:25]=[CH:26][C:19]([F:18])=[CH:20][CH:21]=1

참가 물질

5

반응물 3

HCID 96024-Fluorobenzyl chlorideHCID 11430Potassium CarbonateHCID 949042-Chloroadenine

생성물 1

HCID 115146366-Amino-2-chloro-9-(4-fluorobenzyl)purine수율 1,970.7%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

6-Amino-2-chloropurine (5.02 g) and potassium carbonate (5 g, 36 mmol) were suspended in DMF (200 ml) and thereto was added 4-fluorobenzyl chloride (5 ml, 42 mmol). The mixture was stirred at room temperature for 3 hours. The reaction mixture was concentrated in vacuo to dryness, and to the residue was added water. The mixture was extracted with chloroform and the organic layer was washed with water, dried on sodium sulfate and concentrated in vacuo to dryness. The residue was purified with silica gel chromatography (2% methanol/chloroform) to give the subject compound (162 g).

후처리

  1. concentrationThe reaction mixture was concentrated in vacuo to dryness
  2. additionto the residue was added water
  3. extractionThe mixture was extracted with chloroform
  4. washthe organic layer was washed with water
  5. customdried on sodium sulfate
  6. concentrationconcentrated in vacuo to dryness
  7. customThe residue was purified with silica gel chromatography (2% methanol/chloroform)

출처 및 근거

ORD 기록
ord-de60888fa9cc4327bb7238ebcbcc63fe
출처 데이터셋
uspto-grants-2001_12
특허 번호
US06329381B1

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