Potassium Carbonate → HCID 18366617、化合物

HRID 379578ノート

反応式

HRID 379578 の反応式
C(=O)([O-])[O-].[K+].[K+].[CH3:7][N:8]1[C:13](=[O:14])[C:12]2[CH:15]=[CH:16][S:17][C:11]=2[NH:10][C:9]1=[O:18].[CH:19]1([CH2:22]Br)[CH2:21][CH2:20]1>CN(C)C=O.O>[CH3:7][N:8]1[C:13](=[O:14])[C:12]2[CH:15]=[CH:16][S:17][C:11]=2[N:10]([CH2:22][CH:19]2[CH2:21][CH2:20]2)[C:9]1=[O:18]

参加物

6

反応物 3

HCID 11430Potassium CarbonateHCID 81503BromomethylcyclopropaneHCID 15085573HCID 15085573、化合物

生成物 1

HCID 18366617HCID 18366617、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

Potassium carbonate (1.0 g) was added to a mixture of 3-methylthieno[2,3-d]pyrimidine-2,4(1H,3H)-dione (400 mg; J. Chem. Soc. Perkin Trans.1; 1980; 1853) and cyclopropylmethyl bromide (1.0 ml) in dry dimethylformamide (15 ml). The solution was stirred at room temperature for 20 hours and was then diluted with water and extracted thrice with diethyl ether. The combined organic extracts were washed with brine, then dried, filtered and evaporated. The residue was purified by column chromatography over silica, eluting with ethyl acetate: isohexane (1:4) to give the subtitle compound (180 mg).

後処理

  1. extractionextracted thrice with diethyl ether
  2. washThe combined organic extracts were washed with brine
  3. customdried
  4. filtrationfiltered
  5. customevaporated
  6. customThe residue was purified by column chromatography over silica
  7. washeluting with ethyl acetate: isohexane (1:4)

出典と根拠

ORDレコード
ord-ee27424c39fd47c595507e3c3bc6ca53
出典データセット
uspto-grants-2001_10
特許番号
US06300334B1

反応ノート

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