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

HRID 1666198ノート

反応式

HRID 1666198 の反応式
[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]

参加物

7

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

実験手順

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%

後処理

  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

出典と根拠

ORDレコード
ord-aeb930831a124e69ad5924a36ad1318d
出典データセット
uspto-grants-2011_10
特許番号
US08044056B2

反応ノート

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