Potassium Carbonate → 4-[7-(2-Butynyl)-3-methoxycarbonylmethyl-2,6-dioxo-2,3,6,7-tetrahydro-1H-purin-8-yl]piperazine-1-carboxylic acid tert-butyl ester

HRID 1792062노트

반응식

HRID 1792062 반응식
[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][N:11]([C:14]2[N:22]([CH2:23][C:24]#[C:25][CH3:26])[C:21]3[C:20](=[O:27])[NH:19][C:18](=[O:28])[NH:17][C:16]=3[N:15]=2)[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].C(=O)([O-])[O-].[K+].[K+].Br[CH2:36][C:37]([O:39][CH3:40])=[O:38]>CN(C)C=O.C(OCC)(=O)C>[C:1]([O:5][C:6]([N:8]1[CH2:9][CH2:10][N:11]([C:14]2[N:22]([CH2:23][C:24]#[C:25][CH3:26])[C:21]3[C:20](=[O:27])[NH:19][C:18](=[O:28])[N:17]([CH2:36][C:37]([O:39][CH3:40])=[O:38])[C:16]=3[N:15]=2)[CH2:12][CH2:13]1)=[O:7])([CH3:4])([CH3:2])[CH3:3]

참가 물질

6

반응물 3

HCID 11430Potassium CarbonateHCID 60984Methyl bromoacetateHCID 235369444-[7-(2-Butynyl)-2,6-dioxo-2,3,6,7-tetrahydro-1H-purin-8-yl]piperazine-1-carboxylic acid tert-butyl ester

생성물 1

HCID 235369464-[7-(2-Butynyl)-3-methoxycarbonylmethyl-2,6-dioxo-2,3,6,7-tetrahydro-1H-purin-8-yl]piperazine-1-carboxylic acid tert-butyl ester

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매

실험 절차

4-[7-(2-Butynyl)-2,6-dioxo-2,3,6,7-tetrahydro-1H-purin-8-yl]piperazine-1-carboxylic acid tert-butyl ester (50 mg) and potassium carbonate (20 mg) were dissolved in N,N-dimethylformamide (1.5 ml) and methyl bromoacetate (14 μl) was added to the solution while cooling on ice. After the mixture was stirred at room temperature overnight, the mixture was diluted with ethyl acetate, washed with water, and dried over anhydrous magnesium sulfate. After the organic layer was concentrated by distillation, the residue was purified by silica gel column chromatography to give 26 mg of the title compound from the elution fraction of hexane-ethyl acetate (1:1).

후처리

  1. temperaturewhile cooling on ice
  2. washwashed with water
  3. dry with materialdried over anhydrous magnesium sulfate
  4. concentrationAfter the organic layer was concentrated by distillation
  5. customthe residue was purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-67c84adddfe04c56b3175c19f53c7f99
출처 데이터셋
uspto-grants-2006_07
특허 번호
US07074798B2

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