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Trimethylsilyldiazomethane → 7-Isopropyl-9-methoxy-3,4-dihydro-2H-pyrazino[1,2-c]pyrimidine-1,6,8(7H)-trione

HRID 1162813
ノート
印刷プレビュー

反応式

HRID 1162813 の反応式
[OH:1][C:2]1[C:7](=[O:8])[N:6]([CH:9]([CH3:11])[CH3:10])[C:5](=[O:12])[N:4]2[CH2:13][CH2:14][NH:15][C:16](=[O:17])[C:3]=12.[CH3:18][Si](C=[N+]=[N-])(C)C>CO.CCOCC>[CH:9]([N:6]1[C:7](=[O:8])[C:2]([O:1][CH3:18])=[C:3]2[C:16](=[O:17])[NH:15][CH2:14][CH2:13][N:4]2[C:5]1=[O:12])([CH3:10])[CH3:11]
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 2

HCID 167693TrimethylsilyldiazomethaneHCID 684329449-Hydroxy-7-isopropyl-3,4-dihydro-2H-pyrazino[1,2-c]pyrimidine-1,6,8(7H)-trione

生成物 1

HCID 684325887-Isopropyl-9-methoxy-3,4-dihydro-2H-pyrazino[1,2-c]pyrimidine-1,6,8(7H)-trione

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 3283Diethyl Ether溶媒

実験手順

To a solution of 9-hydroxy-7-isopropyl-3,4-dihydro-2H-pyrazino[1,2-c]pyrimidine-1,6,8(7H)-trione (1.0 g, 4.2 mmol) in MeOH (30 mL) was added trimethylsilyldiazomethane (7 mL of a 2.0 M solution in ether, 14 mmol). The mixture was stirred at ambient temperature for 24 h. The solvent was removed in vacuo and the residue was triturated in MeOH and the solid was collected by filtration to give the title compound as a solid. HPLC RT=2.07 min (Method A); ES MS (M+H)=254; 1H NMR (400 MHz, DMSO-d6) δ 8.64 (2, 1H), 5.03 (septet, J=7 Hz, 1H), 3.86 (m, 2H), 3.66 (s, 3H), 3.37 (m, 2H), 1.38 (d, J=7 Hz, 6H).

後処理

  1. customThe solvent was removed in vacuo
  2. customthe residue was triturated in MeOH
  3. filtrationthe solid was collected by filtration

出典と根拠

ORDレコード
ord-e783733cad5e4304922ea4b4544d7991
出典データセット
uspto-grants-2010_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07820680B2

反応ノート

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