Triethylamine → HCID 59750346、化合物

HRID 499343ノート

反応式

HRID 499343 の反応式
[C:1]([O:10]C)(=O)[C:2]1[C:3](=[CH:5][CH:6]=[CH:7][CH:8]=1)[SH:4].[CH:12]([O:15][C:16]1[CH:21]=[CH:20][C:19]([C:22]#[N:23])=[CH:18][N:17]=1)([CH3:14])[CH3:13].C(N(CC)CC)C>C1(C)C=CC=CC=1>[CH:12]([O:15][C:16]1[N:17]=[CH:18][C:19]([C:22]2[S:4][C:3]3[CH:5]=[CH:6][CH:7]=[CH:8][C:2]=3[C:1](=[O:10])[N:23]=2)=[CH:20][CH:21]=1)([CH3:14])[CH3:13]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 21009Benzoic acid, 2-mercapto-, methyl esterHCID 229393206-Isopropoxynicotinonitrile

生成物 1

HCID 59750346HCID 59750346、化合物収率 30%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

A mixture of methyl thiosalicylate (1.85 g, 11.0 mmol), 2-isopropoxy-5-cyanopyridine (1.62 g, 10.0 mmol), triethylamine (1.80 ml, 12.9 mmol) and toluene (10 ml) was refluxed under nitrogen atmosphere for 30 hrs. The reaction mixture was concentrated. The residue was subjected to a silica gel column chromatography, eluted with ethyl acetate-hexane (2:1, v/v) and recrystallized from ethyl acetate-isopropylether to give the titled compound (0.89 g, 30%).

後処理

  1. temperaturewas refluxed under nitrogen atmosphere for 30 hrs
  2. concentrationThe reaction mixture was concentrated
  3. washeluted with ethyl acetate-hexane (2:1
  4. customv/v) and recrystallized from ethyl acetate-isopropylether

出典と根拠

ORDレコード
ord-0d40247de0f64bc3a5a469e787a0f09e
出典データセット
uspto-grants-2010_08
特許番号
US07767665B2

反応ノート

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