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

HRID 65190

반응식

HRID 65190 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 62761-Pentanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-446e8a80fd7642449b2d5bff95ba4b59
출처 데이터셋
uspto-grants-1986_09
특허 번호
US04613601

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