3-(Piperazin-1-yl)propane-1,2-diol → 3-[4-(2,3-Dihydroxypropyl)piperazin-1-yl]pyrazine-2-carboxylic acid methyl ester dihydrochloride

HRID 231777ノート

反応式

HRID 231777 の反応式
[OH:1][CH:2]([CH2:10][OH:11])[CH2:3][N:4]1[CH2:9][CH2:8][NH:7][CH2:6][CH2:5]1.[CH3:12][O:13][C:14]([C:16]1[C:21]([Cl:22])=[N:20][CH:19]=[CH:18][N:17]=1)=[O:15]>O1CCOCC1>[ClH:22].[ClH:22].[CH3:12][O:13][C:14]([C:16]1[C:21]([N:7]2[CH2:8][CH2:9][N:4]([CH2:3][CH:2]([OH:1])[CH2:10][OH:11])[CH2:5][CH2:6]2)=[N:20][CH:19]=[CH:18][N:17]=1)=[O:15]

参加物

4

反応物 2

HCID 1110023-(Piperazin-1-yl)propane-1,2-diolHCID 1519497Methyl 3-chloropyrazine-2-carboxylate

生成物 1

HCID 678617893-[4-(2,3-Dihydroxypropyl)piperazin-1-yl]pyrazine-2-carboxylic acid methyl ester dihydrochloride

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

Grams 20.5 of 1-(2,3-dihydroxypropyl)piperazine and 11 g of 3-chloropyrazine-2-carboxylic acid methyl ester in 100 ml dioxane were refluxed for one hour. The reaction mixture was cooled and settled, the solvent evaporated and the obtained residue dissolved in concentrated hydrochloric acid and the solution diluted with isopropanol until incipient precipitation. After resting, 12.7 g of 3-[4-(2,3-dihydroxypropyl)piperazin-1-yl]pyrazine-2-carboxylic acid methyl ester dihydrochloride melting at 195°-197° C. (with decomposition), were obtained.

後処理

  1. temperatureThe reaction mixture was cooled
  2. customthe solvent evaporated
  3. dissolutionthe obtained residue dissolved in concentrated hydrochloric acid
  4. additionthe solution diluted with isopropanol until incipient precipitation

出典と根拠

ORDレコード
ord-3379b5f1f1cf4f3ba8ffe7ee21144da1
出典データセット
uspto-grants-1989_07
特許番号
US04849422

反応ノート

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