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

HRID 562714노트

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HRID 562714 반응식
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]

참가 물질

5

반응물 3

HCID 80061-Bromo-3-chloropropaneHCID 11430Potassium CarbonateHCID 178448879HCID 178448879, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
50 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-c6548827ab8c4d8d81743140c778cdb5
출처 데이터셋
uspto-grants-2011_11
특허 번호
US08067426B2

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