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Potassium Carbonate → HCID 13423480、化合物

HRID 2164452
ノート
印刷プレビュー

反応式

HRID 2164452 の反応式
[NH2:1][C:2]1[O:3][N:4]=[C:5]2[C:10]=1[C:9](=[O:11])[N:8]([CH3:12])[C:7](=[O:13])[N:6]2[CH3:14].[CH2:15](I)[CH2:16][CH3:17].C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O>[CH3:12][N:8]1[C:9](=[O:11])[C:10]2=[C:2]([NH:1][CH2:15][CH2:16][CH3:17])[O:3][N:4]=[C:5]2[N:6]([CH3:14])[C:7]1=[O:13]
参加物反応条件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 11430Potassium CarbonateHCID 336431-IodopropaneHCID 126779883-Amino-5,7-dimethyl[1,2]oxazolo[3,4-d]pyrimidine-4,6(5H,7H)-dione

生成物 1

HCID 13423480HCID 13423480、化合物収率 30.4%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
100 °C

実験手順

A mixture of 0.588 g of 3-amino-5,7-dimethyl-isoxazolo[3,4-d]pyrimidine-4,6(5H,7H)-dione, 15 ml of dimethylformamide, 2.5 g of propyl iodide and 1.0 g of potassium carbonate was stirred at 100° C. for 3 hours. From the reaction solution was removed the solvent under reduced pressure. To the residue was added water, which was subjected to extraction with chloroform. The chloroform layer was taken and dried over anhydrous sodium sulfate, from which was removed the solvent. The resultant residue was chromatographed on a column of silica gel (30 g), and the column was eluted with chloroform:acetone:formic acid (20:1:0.1). From the elute was recovered the desired compound, which was recrystallized from isopropyl ether-acetone to give 0.217 g of colorless prisms, melting point: 164°-166° C.

後処理

  1. customFrom the reaction solution was removed the solvent under reduced pressure
  2. additionTo the residue was added water, which
  3. extractionwas subjected to extraction with chloroform
  4. dry with materialdried over anhydrous sodium sulfate, from which
  5. customwas removed the solvent
  6. customThe resultant residue was chromatographed on a column of silica gel (30 g)
  7. washthe column was eluted with chloroform:acetone:formic acid (20:1:0.1)
  8. customFrom the elute was recovered the desired compound, which
  9. customwas recrystallized from isopropyl ether-acetone

出典と根拠

ORDレコード
ord-2a283261039e418397ce59c0010809d2
出典データセット
uspto-grants-1985_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04504662

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート