1-Bromo-3-chloropropane → N2-Butyl-9-(3-chloropropyl)-8-(methyloxy)-9H-purine-2,6-diamine

HRID 562714ノート

反応式

HRID 562714 の反応式
FC(F)(F)C(O)=O.[CH2:8]([NH:12][C:13]1[N:21]=[C:20]2[C:16]([N:17]=[C:18]([O:22][CH3:23])[NH:19]2)=[C:15]([NH2:24])[N:14]=1)[CH2:9][CH2:10][CH3:11].C(=O)([O-])[O-].[K+].[K+].Br[CH2:32][CH2:33][CH2:34][Cl:35]>CN(C=O)C>[CH2:8]([NH:12][C:13]1[N:21]=[C:20]2[C:16]([N:17]=[C:18]([O:22][CH3:23])[N:19]2[CH2:32][CH2:33][CH2:34][Cl:35])=[C:15]([NH2:24])[N:14]=1)[CH2:9][CH2:10][CH3:11]

参加物

5

反応物 3

HCID 80061-Bromo-3-chloropropaneHCID 11430Potassium CarbonateHCID 178448879HCID 178448879、化合物

生成物 1

HCID 59252611N2-Butyl-9-(3-chloropropyl)-8-(methyloxy)-9H-purine-2,6-diamine

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
50 °C

実験手順

N2-Butyl-8-(methyloxy)-9H-purine-2,6-diamine trifluoroacetate (701 mg, 2.001 mmol) and potassium carbonate (690 mg, 4.99 mmol) were suspended in DMF (10 ml) and the mixture heated at 50° C. under nitrogen for 2 hours. The mixture was allowed to cool and then 1-bromo-3-chloropropane (198 μl, 2.002 mmol) was added and the reaction mixture stirred at ambient temperature overnight. After 16 hours the reaction mixture was partitioned between water and DCM (25 ml of each). The aqueous phase was extracted with further DCM (2×20 ml). The combined DCM extracts were dried over magnesium sulphate and concentrated in vacuo to give the impure title compound as a pale yellow oil with some solid present (0.76 g) which was used without further purification.

後処理

  1. temperatureto cool
  2. customAfter 16 hours the reaction mixture was partitioned between water and DCM (25 ml of each)
  3. extractionThe aqueous phase was extracted with further DCM (2×20 ml)
  4. dry with materialThe combined DCM extracts were dried over magnesium sulphate
  5. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-c6548827ab8c4d8d81743140c778cdb5
出典データセット
uspto-grants-2011_11
特許番号
US08067426B2

反応ノート

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