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1-Benzylpiperazine → HCID 13384070, 화합물

HRID 371467
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HRID 371467 반응식
Br[C:2]1[C:3](=[O:12])[NH:4][C:5](=[O:11])[NH:6][C:7]=1[CH2:8][CH2:9][CH3:10].[F-].[K+].[CH2:15]([N:22]1[CH2:27][CH2:26][NH:25][CH2:24][CH2:23]1)[C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1>C(O)C>[C:16]1([CH2:15][N:22]2[CH2:23][CH2:24][N:25]([C:2]3[C:3](=[O:12])[NH:4][C:5](=[O:11])[NH:6][C:7]=3[CH2:8][CH2:9][CH3:10])[CH2:26][CH2:27]2)[CH:17]=[CH:18][CH:19]=[CH:20][CH:21]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 759941-BenzylpiperazineHCID 522689Potassium FluorideHCID 133840665-Bromo-6-propylpyrimidine-2,4(1H,3H)-dione

생성물 1

HCID 13384070HCID 13384070, 화합물수율 58.6%

시약·촉매·용매 1

HCID 702Ethanol용매

반응 조건

온도
140 °C

실험 절차

A mixture of 53.3 g (0.229 mole) of 5-bromo-6-propyl-2,4(1H,3H)pyrimidinedione and 23.7 g (0.252 mole) of anhydrous potassium fluoride in 176 ml (1.0 mole) of 1-benzylpiperazine was heated under reflux at 140° C. for 14 hours. The reaction mixture was cooled to 80° C. and 100 ml of ethanol was added. The mixture was poured into one liter of ice water. The solid was collected and washed with one liter of water. Recrystallization from ethanol and drying in vacuo at 59° C. for 16 hours gave 44.1 g of the product as an off-white solid; mp 233°-235° C.

후처리

  1. temperaturewas heated
  2. temperatureThe reaction mixture was cooled to 80° C.
  3. customThe solid was collected
  4. washwashed with one liter of water
  5. customRecrystallization from ethanol
  6. customdrying in vacuo at 59° C. for 16 hours

출처 및 근거

ORD 기록
ord-93e95a1eae524b12b278022f2569e32a
출처 데이터셋
uspto-grants-1985_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04532240

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