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

HRID 231777노트

반응식

HRID 231777 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-3379b5f1f1cf4f3ba8ffe7ee21144da1
출처 데이터셋
uspto-grants-1989_07
특허 번호
US04849422

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