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Methanol → HCID 69155257, 화합물

HRID 1355410
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HRID 1355410 반응식
[CH3:1][N:2]1[C:10]2[N:9]=[C:8]3[NH:11][CH2:12][CH2:13][N:7]3[C:6]=2[C:5](=[O:14])[N:4]([CH2:15][CH2:16][CH2:17][CH2:18][C@H:19]([O:21][Si:22]([C:25]([CH3:28])([CH3:27])[CH3:26])([CH3:24])[CH3:23])[CH3:20])[C:3]1=[O:29].[C:30](OC(=O)C)(=[O:32])[CH3:31].CO>CN(C)C1C=CN=CC=1.ClCCl>[C:30]([N:11]1[C:8]2=[N:9][C:10]3[N:2]([CH3:1])[C:3](=[O:29])[N:4]([CH2:15][CH2:16][CH2:17][CH2:18][C@H:19]([O:21][Si:22]([C:25]([CH3:28])([CH3:27])[CH3:26])([CH3:23])[CH3:24])[CH3:20])[C:5](=[O:14])[C:6]=3[N:7]2[CH2:13][CH2:12]1)(=[O:32])[CH3:31]
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참가 물질

6

반응물 3

HCID 887MethanolHCID 7918Acetic AnhydrideHCID 136368766HCID 136368766, 화합물

생성물 1

HCID 69155257HCID 69155257, 화합물수율 67%

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매HCID 6344Dichloromethane용매

실험 절차

To a stirring mixture of (R)-7,8-dihydro-1-methyl-3-(5-tert-butyldimethylsilyloxyhexyl)-1H-imidazo[2,1-f]-purine-2,4(3H,6H)-dione (280 mg, 0.65 mmol) and p-dimethylaminopyridine (160 mg, 1.30 mmol) in dichloromethane (10 ml) was added acetic anhydride (100 mg, 0.98 mmol). After stirring at room temperature for 2 hours, the reaction mixture was treated with methanol. After concentration under reduced pressure, the residue was purified by column chromatography on silica gel eluting with ethyl acetate to provide (R)-8-acetyl-7,8-dihydro-1-methyl-3-(5-tert-butyldimethylsilyloxyhexyl)-1H-imidazo[2,1-f]-purine-2,4(3H,6H)-dione (200 mg, 67% yield) as a white powder.

후처리

  1. concentrationAfter concentration under reduced pressure
  2. customthe residue was purified by column chromatography on silica gel eluting with ethyl acetate

출처 및 근거

ORD 기록
ord-76a72f4c99644472a8c2af594d460c1d
출처 데이터셋
uspto-grants-2003_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06586429B2

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