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4-Fluorobenzaldehyde → HCID 54525922, 화합물

HRID 1596229
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HRID 1596229 반응식
Cl.Cl.[C:3]([N:6]1[CH2:11][CH2:10][N:9]([NH2:12])[CH2:8][CH2:7]1)(=[O:5])[CH3:4].[F:13][C:14]1[CH:21]=[CH:20][C:17]([CH:18]=O)=[CH:16][CH:15]=1>C(O)C.C(N(CC)CC)C>[C:3]([N:6]1[CH2:11][CH2:10][N:9]([N:12]=[CH:18][C:17]2[CH:20]=[CH:21][C:14]([F:13])=[CH:15][CH:16]=2)[CH2:8][CH2:7]1)(=[O:5])[CH3:4]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 680234-FluorobenzaldehydeHCID 21701657HCID 21701657, 화합물

생성물 1

HCID 54525922HCID 54525922, 화합물

시약·촉매·용매 2

HCID 702Ethanol용매HCID 8471Triethylamine용매

반응 조건

온도
80 °C

실험 절차

To a solution of 1-acetyl-4-aminopiperazine dihydrochloride (300 mg) in ethanol (10 ml) and triethylamine (0.78 ml) was added p-fluorobenzaldehyde (0.164 ml), and the mixture was heated at 80° C. for 2 hours. After removal of the solvent in vacuo, the residue was triturated with ethyl acetate and water. The organic layer was separated, dried over magnesium sulfate, and concentrated. The residue was crystallized from diisopropyl ether to give 1-acetyl-4-(4-fluorobenzylidene)aminopiperazine (0.15 g).

후처리

  1. customAfter removal of the solvent in vacuo
  2. customthe residue was triturated with ethyl acetate and water
  3. customThe organic layer was separated
  4. dry with materialdried over magnesium sulfate
  5. concentrationconcentrated
  6. customThe residue was crystallized from diisopropyl ether

출처 및 근거

ORD 기록
ord-691f23435a8f4e659064e673779ee133
출처 데이터셋
uspto-grants-2001_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06291464B1

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