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Hydrochloric Acid → 4-(5-(3-Cyanophenyl)-1,3-dimethyl-2,4-dioxo-3,4-dihydro-1H-pyrrolo[3,4-d]pyrimidin-6(2H)-yl)-N-methoxy-N-methylbutanamide

HRID 2201212
ノート
印刷プレビュー

反応式

HRID 2201212 の反応式
C(P1(=O)OP(CCC)(=O)OP(CCC)(=O)O1)CC.Cl.CC[N:22]([CH:26](C)C)C(C)C.[C:29]([C:31]1[CH:32]=[C:33]([C:37]2[N:38]([CH2:50][CH2:51][CH2:52][C:53]([O-])=[O:54])[CH:39]=[C:40]3[C:45]=2[C:44](=[O:46])[N:43]([CH3:47])[C:42](=[O:48])[N:41]3[CH3:49])[CH:34]=[CH:35][CH:36]=1)#[N:30].[Li+].CN([CH:60]=[O:61])C>>[C:29]([C:31]1[CH:32]=[C:33]([C:37]2[N:38]([CH2:50][CH2:51][CH2:52][C:53]([N:22]([O:61][CH3:60])[CH3:26])=[O:54])[CH:39]=[C:40]3[C:45]=2[C:44](=[O:46])[N:43]([CH3:47])[C:42](=[O:48])[N:41]3[CH3:49])[CH:34]=[CH:35][CH:36]=1)#[N:30]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 5

HCID 313Hydrochloric AcidHCID 6228DimethylformamideHCID 81531DiisopropylethylamineHCID 111923Propylphosphonic anhydrideHCID 86723451Lithium 4-(5-(3-cyanophenyl)-1,3-dimethyl-2,4-dioxo-3,4-dihydro-1H-pyrrolo[3,4-d]pyrimidin-6(2H)-yl)butanoate

生成物 1

HCID 86723452
4-(5-(3-Cyanophenyl)-1,3-dimethyl-2,4-dioxo-3,4-dihydro-1H-pyrrolo[3,4-d]pyrimidin-6(2H)-yl)-N-methoxy-N-methylbutanamide

実験手順

T3P® (31.3 ml, 52.6 mmol) was added dropwise to a solution of N,O-dimethyllhydroxylamine hydrochloride (2.70 g, 27.6 mmol), DIPEA (18.39 ml, 105 mmol) and lithium 4-(5-(3-cyanophenyl)-1,3-dimethyl-2,4-dioxo-3,4-dihydro-1H-pyrrolo[3,4-d]pyrimidin-6(2H)-yl)butanoate (9.8 g, 26.3 mmol) in DMF (263 mL). The mixture was stirred at room temperature for 40 minutes and quenched with water (250 mL). The resultant precipitate was collected by filtration under reduced pressure to afford the title compound.

後処理

  1. customquenched with water (250 mL)
  2. filtrationThe resultant precipitate was collected by filtration under reduced pressure

出典と根拠

ORDレコード
ord-f03ca06b77654e51b53e50b8de2d2f4e
出典データセット
uspto-grants-2016_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09359381B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート