1-Bromopropane → HCID 19001410、化合物

HRID 2259558ノート

反応式

HRID 2259558 の反応式
[NH:1]1[C:5]([C:6]2[C:11](=[O:12])[N:10]3[CH:13]=[CH:14][CH:15]=[CH:16][C:9]3=[N:8][CH:7]=2)=[N:4][N:3]=[N:2]1.C(=O)([O-])[O-].[K+].[K+].[CH2:23](Br)[CH2:24][CH3:25]>CN(C)C=O>[CH2:23]([N:3]1[N:2]=[N:1][C:5]([C:6]2[C:11](=[O:12])[N:10]3[CH:13]=[CH:14][CH:15]=[CH:16][C:9]3=[N:8][CH:7]=2)=[N:4]1)[CH2:24][CH3:25]

参加物

5

反応物 3

HCID 78401-BromopropaneHCID 11430Potassium CarbonateHCID 178515422HCID 178515422、化合物

生成物 1

HCID 19001410HCID 19001410、化合物収率 31.3%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
90 °C

実験手順

A mixture of 0.4 g (0.00187 moles) of 3-(1H-tetrazol-5-yl)-4-oxo-4H-pyrido[1,2-a]pyrimidine, 15 ml of dimethylformamide, 0.25 g (0.00187 moles) of anhydrous potassium carbonate and 0.34 ml (0.00374 moles) of propyl bromide was stirred at 90° C. for 1 hour. The hot dark brown solution was filtered, and the filtrate was evaporated. The dark brown oily residue, which is the mixture of the title compounds, started to crystallize. To the oily crystals 10 ml of ethanol were added, and the crystals were collected. 0.15 g (31.3%) of 3-(2-propyl-2H-tetrazol-5-yl)-4-oxo-4H-pyrido[1,2 -a]pyrimidine was obtained, in the form of pale-yellow crystals, m.p.: 115°-116° C.

後処理

  1. filtrationThe hot dark brown solution was filtered
  2. customthe filtrate was evaporated
  3. additionthe mixture of the title compounds
  4. customto crystallize
  5. additionTo the oily crystals 10 ml of ethanol were added
  6. customthe crystals were collected

出典と根拠

ORDレコード
ord-60caeacbcae745d2b73080a0aeea5e6d
出典データセット
uspto-grants-1995_12
特許番号
US05475000

反応ノート

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