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

HRID 2269146ノート

反応式

HRID 2269146 の反応式
[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

参加物

5

反応物 3

HCID 96024-Fluorobenzyl chlorideHCID 11430Potassium CarbonateHCID 949042-Chloroadenine

生成物 1

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

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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).

後処理

  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)

出典と根拠

ORDレコード
ord-de60888fa9cc4327bb7238ebcbcc63fe
出典データセット
uspto-grants-2001_12
特許番号
US06329381B1

反応ノート

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