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

HRID 1920664노트

반응식

HRID 1920664 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-879382b092194ee892b0db0e9cbe463d
출처 데이터셋
uspto-grants-2012_05
특허 번호
US08173609B2

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