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Potassium Iodide → HCID 12852065, 화합물

HRID 1248240
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HRID 1248240 반응식
Cl[CH2:2][CH2:3][CH2:4][N:5]1[C:14]2[C:9](=[CH:10][CH:11]=[CH:12][CH:13]=2)[C:8](=[O:15])[NH:7][C:6]1=[O:16].Cl.[F:18][C:19]1[CH:24]=[CH:23][C:22]([C:25]([CH:27]2[CH2:32][CH2:31][NH:30][CH2:29][CH2:28]2)=[O:26])=[CH:21][CH:20]=1.C(=O)([O-])[O-].[Na+].[Na+].[I-].[K+]>O.CC(C)CC(=O)C>[F:18][C:19]1[CH:20]=[CH:21][C:22]([C:25]([CH:27]2[CH2:32][CH2:31][N:30]([CH2:2][CH2:3][CH2:4][N:5]3[C:14]4[C:9](=[CH:10][CH:11]=[CH:12][CH:13]=4)[C:8](=[O:15])[NH:7][C:6]3=[O:16])[CH2:29][CH2:28]2)=[O:26])=[CH:23][CH:24]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 4875Potassium IodideHCID 10340Sodium CarbonateHCID 3084438p-Fluorophenyl 4-piperidyl ketone hydrochlorideHCID 134765441-(3-Chloropropyl)quinazoline-2,4(1H,3H)-dione

생성물 1

HCID 12852065HCID 12852065, 화합물수율 18.5%

시약·촉매·용매 2

HCID 962
Water
용매
2회
HCID 7909Methyl Isobutyl Ketone용매

실험 절차

A mixture of 3.6 parts of 1-(3-chloropropyl)-2,4(1H,3H)-quinazolinedione, 3.02 parts of (4-fluorophenyl)(4-piperidinyl)methanone hydrochloride, 3.7 parts of sodium carbonate, 0.1 parts of potassium iodide and 120 parts of 4-methyl-2-pentanone is stirred and refluxed overnight using a water-separator. The reaction mixture is cooled, water is added and the layers are separated. The organic phase is dried, filtered and concentrated to a small volume. After cooling the concentrate, the precipitated product is filtered off and crystallized from 2-propanol, yielding 1.3 parts (18.5%) of 1-[3-[4-(4-fluorobenzoyl)-1-piperidinyl]propyl]-2,4(1H,3H)-quinazolinedione; mp. 192.9° C.

후처리

  1. temperaturerefluxed overnight
  2. temperatureThe reaction mixture is cooled
  3. customthe layers are separated
  4. customThe organic phase is dried
  5. filtrationfiltered
  6. concentrationconcentrated to a small volume
  7. temperatureAfter cooling the concentrate
  8. filtrationthe precipitated product is filtered off
  9. customcrystallized from 2-propanol

출처 및 근거

ORD 기록
ord-df63f86af4c74c21a3eb66c2ebfc09c7
출처 데이터셋
uspto-grants-1985_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04522945

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