Water → 9-(3-Bromopropyl)-2-butoxy-8-methoxy-9H-purin-6-amine

HRID 1666198노트

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HRID 1666198 반응식
[CH2:1]([O:5][C:6]1[N:14]=[C:13]2[C:9]([NH:10][C:11]([O:15][CH3:16])=[N:12]2)=[C:8]([NH2:17])[N:7]=1)[CH2:2][CH2:3][CH3:4].[Br:18][CH2:19][CH2:20][CH:21](Br)C.C(=O)([O-])[O-].[K+].[K+].O>CN(C)C=O.C(OCC)(=O)C>[Br:18][CH2:19][CH2:20][CH2:21][N:12]1[C:11]([O:15][CH3:16])=[N:10][C:9]2[C:13]1=[N:14][C:6]([O:5][CH2:1][CH2:2][CH2:3][CH3:4])=[N:7][C:8]=2[NH2:17]

참가 물질

7

반응물 4

HCID 962WaterHCID 78891,3-DibromobutaneHCID 11430Potassium CarbonateHCID 574571342-(Butyloxy)-8-(methyloxy)-9H-purin-6-amine

생성물 1

HCID 231584909-(3-Bromopropyl)-2-butoxy-8-methoxy-9H-purin-6-amine수율 71%

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매

실험 절차

To a solution of 2-butoxy-8-methoxyadenine (5 g, 14.2 mmol) in dimethylformamide (50 ml) were added 1,3-dibromobutane (7.2 ml) and potassium carbonate (9.2 g), and the mixture was stirred at room temperature for 1.5 hour. Water (200 ml) and ethyl acetate (75 ml) were added thereto, and the mixture was extracted, and further extracted with ethyl acetate (75 ml) twice. The organic layers were combined, dried over magnesium sulfate, filtered, and the solvent was distilled off under reduced pressure. To the residue was added diethyl ether (25 ml), and the precipitated crystals were collected by filtration, washed with ether (5 ml), and dried to give the subtitle compound (3.6 g) as a white solid. Yield: 71%

후처리

  1. extractionthe mixture was extracted
  2. extractionfurther extracted with ethyl acetate (75 ml) twice
  3. dry with materialdried over magnesium sulfate
  4. filtrationfiltered
  5. distillationthe solvent was distilled off under reduced pressure
  6. additionTo the residue was added diethyl ether (25 ml)
  7. filtrationthe precipitated crystals were collected by filtration
  8. washwashed with ether (5 ml)
  9. customdried

출처 및 근거

ORD 기록
ord-aeb930831a124e69ad5924a36ad1318d
출처 데이터셋
uspto-grants-2011_10
특허 번호
US08044056B2

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