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Benzaldehyde → 6-Amino-9-(3-{benzyl[2-(dimethylamino)ethyl]amino}propyl)-2-butoxy-7,9-dihydro-8h-purin-8-one

HRID 562494
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인쇄 미리보기

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HRID 562494 반응식
Cl.[NH2:2][C:3]1[N:11]=[C:10]([O:12][CH2:13][CH2:14][CH2:15][CH3:16])[N:9]=[C:8]2[C:4]=1[NH:5][C:6](=[O:26])[N:7]2[CH2:17][CH2:18][CH2:19][NH:20][CH2:21][CH2:22][N:23]([CH3:25])[CH3:24].[CH:27](=O)[C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1.C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+]>CN1C(=O)CCC1.CO>[NH2:2][C:3]1[N:11]=[C:10]([O:12][CH2:13][CH2:14][CH2:15][CH3:16])[N:9]=[C:8]2[C:4]=1[NH:5][C:6](=[O:26])[N:7]2[CH2:17][CH2:18][CH2:19][N:20]([CH2:27][C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1)[CH2:21][CH2:22][N:23]([CH3:25])[CH3:24]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 240BenzaldehydeHCID 5049666Sodium triacetoxyborohydrideHCID 1317292896-Amino-2-butoxy-9-(3-{[2-(dimethylamino)ethyl]amino}propyl)-7,9-dihydro-8H-purin-8-one, hydrochloride

생성물 1

HCID 249646906-Amino-9-(3-{benzyl[2-(dimethylamino)ethyl]amino}propyl)-2-butoxy-7,9-dihydro-8h-purin-8-one수율 59.7%

시약·촉매·용매 2

HCID 887
Methanol
용매
HCID 13387N-methyl-2-pyrrolidone용매

실험 절차

The product from step (iii) (0.1 g) and benzaldehyde (0.0362 g, 0.0347 ml) were combined in NMP (4 mL) and stirred at RT for 15 mins. Sodium triacetoxyborohydride (0.0904 g) was added. The reaction mixture was stirred for 16 h. The reaction mixture was diluted with methanol and purified by RP-prep-HPLC 75:05 NH3:acetonitrile over 15 mins to give title compound (0.068 g)

후처리

  1. stirringThe reaction mixture was stirred for 16 h
  2. custompurified by RP-prep-HPLC 75:05 NH3

출처 및 근거

ORD 기록
ord-3a70e952d2aa4bc686d2f57b9cc4286f
출처 데이터셋
uspto-grants-2011_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08067411B2

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