Potassium Carbonate → Pyrimidine, 2-(4-(1,4-benzodioxin-6-ylmethyl)-1-piperazinyl)-, dihydrochloride

HRID 65190

反応式

HRID 65190 の反応式
[Cl:1][C:2]1[N:7]=[CH:6][CH:5]=[CH:4][N:3]=1.[O:8]1[C:13]2[CH:14]=[CH:15][C:16]([CH2:18][N:19]3[CH2:24][CH2:23][NH:22][CH2:21][CH2:20]3)=[CH:17][C:12]=2[O:11][CH:10]=[CH:9]1.C(=O)([O-])[O-].[K+].[K+]>C(O)CCCC>[ClH:1].[ClH:1].[O:8]1[C:13]2[CH:14]=[CH:15][C:16]([CH2:18][N:19]3[CH2:20][CH2:21][N:22]([C:2]4[N:7]=[CH:6][CH:5]=[CH:4][N:3]=4)[CH2:23][CH2:24]3)=[CH:17][C:12]=2[O:11][CH:10]=[CH:9]1

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 744042-ChloropyrimidineHCID 704553951-(6-Benzodioxinyl methyl)piperazine

生成物 1

HCID 3071330Pyrimidine, 2-(4-(1,4-benzodioxin-6-ylmethyl)-1-piperazinyl)-, dihydrochloride収率 156.5%

試薬・触媒・溶媒 1

HCID 62761-Pentanol溶媒

実験手順

A solution of 11.4 g (0.1 mole) of 2-chloropyrimidine and 23.2 g (0.1 mole) of 1-(6-benzodioxinyl methyl)piperazine (oil) in 500 ml of pentanol, as refluxed for 6 hours, in the presence of 13.8 g (0.1 mole) of potassium carbonate. After the completion of the reaction, the so-formed salt was filtered off and the solvent was evaporated under reduced pressure. The so-obtained oily residue (30 g) was dissolved in 160 ml of anhydrous ethanol. After addition of an excess of hydrochloric acid ether solution, the dihydrochloride crystallises. 30 g of 1-(benzodioxin-6-yl methyl)-4-(pyrimidin-2-yl)piperazine dihydrochloride white crystals were finally obtained, melting at 215°-220° C.

後処理

  1. customAfter the completion of the reaction
  2. filtrationthe so-formed salt was filtered off
  3. customthe solvent was evaporated under reduced pressure
  4. dissolutionThe so-obtained oily residue (30 g) was dissolved in 160 ml of anhydrous ethanol
  5. additionAfter addition of an excess of hydrochloric acid ether solution
  6. customthe dihydrochloride crystallises

出典と根拠

ORDレコード
ord-446e8a80fd7642449b2d5bff95ba4b59
出典データセット
uspto-grants-1986_09
特許番号
US04613601

関連ノート

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