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Acetonitrile → Methyl[4-({[3-(6-amino-2-butoxy-8-oxo-7,8-dihydro-9h-purin-9-yl)propyl][(4-methylpiperazin-1-yl)acetyl]amino}methyl)phenyl]acetate

HRID 1095329
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HRID 1095329 반응식
[CH3:1][O:2][C:3](=[O:32])[CH2:4][C:5]1[CH:10]=[CH:9][C:8]([CH2:11][NH:12][CH2:13][CH2:14][CH2:15][N:16]2[C:24](=[O:25])[NH:23][C:22]3[C:17]2=[N:18][C:19]([O:27][CH2:28][CH2:29][CH2:30][CH3:31])=[N:20][C:21]=3[NH2:26])=[CH:7][CH:6]=1.Cl[CH2:34][C:35](Cl)=[O:36].[CH3:38][C:39]#[N:40]>>[CH3:1][O:2][C:3](=[O:32])[CH2:4][C:5]1[CH:10]=[CH:9][C:8]([CH2:11][N:12]([CH2:13][CH2:14][CH2:15][N:16]2[C:24](=[O:25])[NH:23][C:22]3[C:17]2=[N:18][C:19]([O:27][CH2:28][CH2:29][CH2:30][CH3:31])=[N:20][C:21]=3[NH2:26])[C:35](=[O:36])[CH2:34][N:40]2[CH2:8][CH2:11][N:12]([CH3:13])[CH2:38][CH2:39]2)=[CH:7][CH:6]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 6342AcetonitrileHCID 6577Chloroacetyl chlorideHCID 90697362Methyl[4-({[3-(6-amino-2-butoxy-8-oxo-7,8-dihydro-9H-purin-9-yl)propyl]amino}methyl)phenyl]acetate

생성물 1

HCID 23649460Methyl[4-({[3-(6-amino-2-butoxy-8-oxo-7,8-dihydro-9h-purin-9-yl)propyl][(4-methylpiperazin-1-yl)acetyl]amino}methyl)phenyl]acetate

실험 절차

The product from step (ix) (200 mg) was suspended in MeCN. Chloroacetyl chloride (0.02 ml) added and the mixture stirred at rt for 4 h. The mixture was concentrated under reduced pressure, piperazine (0.02 ml) in DMSO (1 ml) was added and the mixture heated at 60° C. for 24 h. The mixture was purified by RPHPLC. Yield 80 mg.

후처리

  1. concentrationThe mixture was concentrated under reduced pressure, piperazine (0.02 ml) in DMSO (1 ml)
  2. additionwas added
  3. temperaturethe mixture heated at 60° C. for 24 h
  4. customThe mixture was purified by RPHPLC

출처 및 근거

ORD 기록
ord-03f4b6d868cd40f4a3fd4ba996801ea4
출처 데이터셋
uspto-grants-2012_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08138172B2

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