Dichlorodimethylsilane → 2,6-Dichloropurine

HRID 969709ノート

反応式

HRID 969709 の反応式
C([N:4]1[CH:12]=[N:11][C:10]2[C:5]1=[N:6][C:7](N)=[N:8][C:9]=2[Cl:13])(=O)C.[Cl:15][Si](Cl)(C)C.N(OCCC(C)C)=O>[Cl-].C([N+](CC)(CC)CC)C.CCCCCCC>[Cl:15][C:7]1[N:6]=[C:5]2[C:10]([NH:11][CH:12]=[N:4]2)=[C:9]([Cl:13])[N:8]=1

参加物

6

反応物 3

HCID 6398DichlorodimethylsilaneHCID 8053Isoamyl NitriteHCID 10149094HCID 10149094、化合物

生成物 1

HCID 53244122,6-Dichloropurine収率 73.8%

試薬・触媒・溶媒 2

HCID 5946Tetraethylammonium Chloride触媒HCID 8900Heptane溶媒

反応条件

温度
55 °C

実験手順

9-Acetyl-2-amino-6-chloropurine (0.50 g, 2.36 mmol), dichlorodimethylsilane (1.01 g, 7.80 mmol), tetraethylammonium chloride (0.025 g, 0.15 mmol) and isoamyl nitrite (0.42 g, 3.54 mmol) were added to heptane (4 ml), and the mixture was heated to 50-60° C. and stirred for 14 hr. After the completion of the reaction, the mixture was filtrated. The obtained crystals were diluted with water (4.0 ml), and the mixture was adjusted to pH 4-5 with a 2M aqueous sodium hydroxide solution. After aging under ice-cooling for 1 hr, the mixture was filtrated, and the obtained crystals were dried under reduced pressure at 80° C. to give a white powder (0.31 g, yield 73.8%) of 2,6-dichloropurine.

後処理

  1. customAfter the completion of the reaction
  2. filtrationthe mixture was filtrated
  3. additionThe obtained crystals were diluted with water (4.0 ml)
  4. temperaturecooling for 1 hr
  5. filtrationthe mixture was filtrated
  6. customthe obtained crystals were dried under reduced pressure at 80° C.

出典と根拠

ORDレコード
ord-a3c9ed2c2092469fbfc92b52a7f6f57a
出典データセット
uspto-grants-2007_12
特許番号
US07307167B2

反応ノート

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