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

HRID 1723443ノート

反応式

HRID 1723443 の反応式
[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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 2631-Butanol溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-5838677f32fb46fd84bcf7fe3a74ba4f
出典データセット
uspto-grants-1989_08
特許番号
US04861785

反応ノート

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