1-Bromo-2-Chloroethane → 9-(2-Chloroethyl)-2,6-diamino-purine

HRID 1920664ノート

反応式

HRID 1920664 の反応式
[NH2:1][C:2]1[N:10]=[C:9]2[C:5]([NH:6][CH:7]=[N:8]2)=[C:4]([NH2:11])[N:3]=1.C(=O)([O-])[O-].[K+].[K+].Br[CH2:19][CH2:20][Cl:21]>CN(C=O)C>[Cl:21][CH2:20][CH2:19][N:8]1[CH:7]=[N:6][C:5]2[C:9]1=[N:10][C:2]([NH2:1])=[N:3][C:4]=2[NH2:11]

参加物

5

反応物 3

HCID 78491-Bromo-2-ChloroethaneHCID 11430Potassium CarbonateHCID 309762,6-Diaminopurine

生成物 1

HCID 668680839-(2-Chloroethyl)-2,6-diamino-purine収率 72%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

10 g (66.6 mmol) 2,6-diaminopurine were suspended under argon in 300 ml DMF and 21.6 g (156.5 mmol) potassium carbonate and 24 ml 1-bromo-2-chloroethane were added. The mixture was stirred for 64 hours at room temperature. The light yellow suspension was filtered and the solids were washed with 30 ml DMF and subsequently triturated with 100 ml water for 30 minutes. The mixture was filtered and the solids were washed with 50 ml water and dried in vacuo to give 10.15 g (72%) of the desired product as a white solid.

後処理

  1. filtrationThe light yellow suspension was filtered
  2. washthe solids were washed with 30 ml DMF
  3. customsubsequently triturated with 100 ml water for 30 minutes
  4. filtrationThe mixture was filtered
  5. washthe solids were washed with 50 ml water
  6. customdried in vacuo

出典と根拠

ORDレコード
ord-879382b092194ee892b0db0e9cbe463d
出典データセット
uspto-grants-2012_05
特許番号
US08173609B2

反応ノート

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