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Ethoxyacetyl chloride → Tert-butyl 2-({7-bromo-3-[(ethoxyacetyl)amino][1,5]naphthyridin-4-yl}amino)-1,1-dimethylethylcarbamate hydrochloride

HRID 598040
ノート
印刷プレビュー

反応式

HRID 598040 の反応式
NC1C2N=C(COCC)N(CC(C)(O)C)C=2C2N=CC(Br)=CC=2N=1.[NH2:25][C:26]1[CH:27]=[N:28][C:29]2[C:34]([C:35]=1[NH:36][CH2:37][C:38]([NH:41][C:42](=[O:48])[O:43][C:44]([CH3:47])([CH3:46])[CH3:45])([CH3:40])[CH3:39])=[N:33][CH:32]=[C:31]([Br:49])[CH:30]=2.[CH2:50]([O:52][CH2:53][C:54]([Cl:56])=[O:55])[CH3:51]>C(#N)C>[ClH:56].[Br:49][C:31]1[CH:30]=[C:29]2[C:34]([C:35]([NH:36][CH2:37][C:38]([NH:41][C:42](=[O:48])[O:43][C:44]([CH3:47])([CH3:46])[CH3:45])([CH3:40])[CH3:39])=[C:26]([NH:25][C:54](=[O:55])[CH2:53][O:52][CH2:50][CH3:51])[CH:27]=[N:28]2)=[N:33][CH:32]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 84189Ethoxyacetyl chlorideHCID 589706811-[4-amino-7-bromo-2-(ethoxymethyl)-1H-imidazo[4,5-c][1,5]naphthyridin-1-yl]-2-methylpropan-2-olHCID 67052529Tert-butyl 2-[(3-amino-7-bromo[1,5]naphthyridin-4-yl)amino]-1,1-dimethylethylcarbamate

生成物 1

HCID 67052443Tert-butyl 2-({7-bromo-3-[(ethoxyacetyl)amino][1,5]naphthyridin-4-yl}amino)-1,1-dimethylethylcarbamate hydrochloride収率 66.9%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒2 回

実験手順

The method described in Part C of the preparation of 1-[4-amino-7-bromo-2-(ethoxymethyl)-1H-imidazo[4,5-c][1,5]naphthyridin-1-yl]-2-methylpropan-2-ol was used to treat tert-butyl 2-[(3-amino-7-bromo[1,5]naphthyridin-4-yl)amino]-1,1-dimethylethylcarbamate (64.0 g, 0.156 mol) with ethoxyacetyl chloride (21.0 g, 0.171 mol) in acetonitrile (640 mL). At the completion of the reaction, additional acetonitrile (200 mL) was added, and the solid product was isolated by filtration, washed with a small volume of acetonitrile, and dried for four hours to provide 55.6 g of tert-butyl 2-({7-bromo-3-[(ethoxyacetyl)amino][1,5]naphthyridin-4-yl}amino)-1,1-dimethylethylcarbamate hydrochloride.

後処理

  1. additionwas added
  2. customthe solid product was isolated by filtration
  3. washwashed with a small volume of acetonitrile
  4. customdried for four hours

出典と根拠

ORDレコード
ord-b2a2df60325045a2a1d2b185d85a9e5a
出典データセット
uspto-grants-2011_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07897609B2

反応ノート

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