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Cyclopropylamine → HCID 14651159, 화합물

HRID 232651
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HRID 232651 반응식
[CH3:1][N:2]1[CH2:7][CH2:6][N:5]([C:8]2[C:13]([F:14])=[C:12]([CH3:15])[C:11]([N+:16]([O-:18])=[O:17])=[C:10](F)[C:9]=2[CH3:20])[CH2:4][CH2:3]1.[F-].[K+].[CH:23]1([NH2:26])[CH2:25][CH2:24]1>CS(C)=O>[CH3:1][N:2]1[CH2:7][CH2:6][N:5]([C:8]2[C:9]([CH3:20])=[C:10]([C:11]([N+:16]([O-:18])=[O:17])=[C:12]([CH3:15])[C:13]=2[F:14])[NH:26][CH:23]2[CH2:25][CH2:24]2)[CH2:4][CH2:3]1
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참가 물질

5

반응물 3

HCID 69828CyclopropylamineHCID 522689Potassium FluorideHCID 23359030HCID 23359030, 화합물

생성물 1

HCID 14651159HCID 14651159, 화합물

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

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온도
100 °C

실험 절차

To 2-(4-methyl-1-piperazinyl)-3,6-difluoro-4-methyl-5-nitrotoluene (1.73 g) are added anhydrous dimethyl sulfoxide (18 ml), potassium fluoride (0.53 g) and cyclopropylamine (2.2 ml) and the mixture is stirred at 100° C. for 23 hours. After cooling, the mixture is poured into ice-water, extracted with dichloromethane and the extract is dried. The solvent is distilled off under reduced pressure and the residue is purified by silica-gel column-chromatography (dichloromethane: methanol=40:1) to give 3-(4-methyl-1-piperazinyl)-4-fluoro-2,5-dimethyl-6-nitro-N-cyclopropylaniline (1.65 g).

후처리

  1. temperatureAfter cooling
  2. extractionextracted with dichloromethane
  3. customthe extract is dried
  4. distillationThe solvent is distilled off under reduced pressure
  5. customthe residue is purified by silica-gel column-chromatography (dichloromethane: methanol=40:1)

출처 및 근거

ORD 기록
ord-91f152fdeec24963a23baeb9b379d8f1
출처 데이터셋
uspto-grants-1997_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05591744

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