Ammonia → HCID 15379780, 화합물

HRID 1736476노트

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HRID 1736476 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([Cl:8])[C:3]=1[CH:9]([CH3:11])[NH2:10].Cl[C:13]1[C:18]([C:19]#[N:20])=[CH:17][CH:16]=[CH:15][N:14]=1.N>CN(C)C(=O)C>[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([Cl:8])[C:3]=1[CH:9]([NH:10][C:13]1[C:18]([C:19]#[N:20])=[CH:17][CH:16]=[CH:15][N:14]=1)[CH3:11]

참가 물질

5

반응물 3

HCID 222AmmoniaHCID 810792-ChloronicotinonitrileHCID 109103151-(2,6-dichlorophenyl)ethanaMine hydrochloride

생성물 1

HCID 15379780HCID 15379780, 화합물수율 41.4%

시약·촉매·용매 1

HCID 31374Dimethylacetamide용매

반응 조건

온도
90 °C

실험 절차

A mixture of 2,6-dichloro-α-methylbenzenemethanamine (0.03 mol) and 2-chloro-3-pyridinecarbonitrile (0.03 mol) in N,N-dimethylacetamide (few drops) was stirred for 20 hours at 90° C. The reaction mixture was cooled and poured out into aqueous ammonia. The mixture was extracted twice with CH2Cl2. The organic layer was separated, washed with water, dried (MgSO4), filtered and the solvent was evaporated. The residue was purified by column chromatography over silica gel (eluent: CH2Cl2 /hexane 50/50). The pure fractions were collected and the solvent was evaporated, yielding 3.6 g (±)-2-[[1-(2,6-dichlorophenyl)ethyl]amino]-3-pyridinecarbonitrile (41.4%); mp. 84.4° C. (comp. 9).

후처리

  1. temperatureThe reaction mixture was cooled
  2. extractionThe mixture was extracted twice with CH2Cl2
  3. customThe organic layer was separated
  4. washwashed with water
  5. dry with materialdried (MgSO4)
  6. filtrationfiltered
  7. customthe solvent was evaporated
  8. customThe residue was purified by column chromatography over silica gel (eluent: CH2Cl2 /hexane 50/50)
  9. customThe pure fractions were collected
  10. customthe solvent was evaporated

출처 및 근거

ORD 기록
ord-d9bb0c7bfded4cbc990a488b09f6663a
출처 데이터셋
uspto-grants-1996_07
특허 번호
US05541215

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