4-Vinylpyridine → N-[1-[2-(4-pyridinyl)ethyl]-4-piperidinyl]-2-benzoxazolamine

HRID 1723443

반응식

HRID 1723443 반응식
[CH:1]([C:3]1[CH:8]=[CH:7][N:6]=[CH:5][CH:4]=1)=[CH2:2].[NH:9]1[CH2:14][CH2:13][CH:12]([NH:15][C:16]2[O:17][C:18]3[CH:24]=[CH:23][CH:22]=[CH:21][C:19]=3[N:20]=2)[CH2:11][CH2:10]1>C(O)CCC>[N:6]1[CH:7]=[CH:8][C:3]([CH2:1][CH2:2][N:9]2[CH2:10][CH2:11][CH:12]([NH:15][C:16]3[O:17][C:18]4[CH:24]=[CH:23][CH:22]=[CH:21][C:19]=4[N:20]=3)[CH2:13][CH2:14]2)=[CH:4][CH:5]=1

참가 물질

4

반응물 2

HCID 75024-VinylpyridineHCID 14575294N-(4-piperidinyl)-2-benzoxazolamine

생성물 1

HCID 14575870N-[1-[2-(4-pyridinyl)ethyl]-4-piperidinyl]-2-benzoxazolamine수율 62%

시약·촉매·용매 1

HCID 2631-Butanol용매

실험 절차

A mixture of 3.2 parts of 4-(1-ethenyl)pyridine, 2.1 parts of N-(4-piperidinyl)-2-benzoxazolamine and 80 parts of 1-butanol was stirred and refluxed for 48 hours. The reaction mixture was evaporated. The residue was purified by column chromatography over silica gel using a mixture of trichloromethane and methanol (97:3 by volume) saturated with ammonia, as eluent. The pure fractions were collected and the eluent was evaporated. The residue was crystallized from 2,2'-oxybispropane, yielding 2 parts (62%) of N-[1-[2-(4-pyridinyl)ethyl]-4-piperidinyl]-2-benzoxazolamine; mp. 146.9° C. (450).

후처리

  1. temperaturerefluxed for 48 hours
  2. customThe reaction mixture was evaporated
  3. customThe residue was purified by column chromatography over silica gel using
  4. additiona mixture of trichloromethane and methanol (97:3 by volume) saturated with ammonia
  5. customThe pure fractions were collected
  6. customthe eluent was evaporated
  7. customThe residue was crystallized from 2,2'-oxybispropane

출처 및 근거

ORD 기록
ord-5838677f32fb46fd84bcf7fe3a74ba4f
출처 데이터셋
uspto-grants-1989_08
특허 번호
US04861785

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