Triethylamine → HCID 68459271、化合物

HRID 499294ノート

反応式

HRID 499294 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].C(O[C:16]1[CH:17]=[CH:18][C:19]([C:22]#N)=[N:20][CH:21]=1)(=O)C.[C:24]([O:27]C1C(C#N)=NC=CC=1)(=[O:26])[CH3:25].[CH2:36]([N:38](CC)CC)C>C1(C)C=CC=CC=1>[C:24]([O:27][CH2:22][C:19]1[CH:18]=[CH:17][C:16]([C:36]2[S:4][C:3]3[CH:5]=[CH:6][CH:7]=[CH:8][C:2]=3[C:1](=[O:10])[N:38]=2)=[CH:21][N:20]=1)(=[O:26])[CH3:25]

参加物

6

反応物 4

HCID 8471TriethylamineHCID 21009Benzoic acid, 2-mercapto-, methyl esterHCID 22939311HCID 22939311、化合物HCID 229393796-Cyanopyridin-3-yl acetate

生成物 1

HCID 68459271HCID 68459271、化合物収率 29%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

A mixture of methyl thiosalicylate (0.58 g, 3.43 mmol), a mixture of 5-acetoxy-2-cyanopyridine and 3-acetoxy-2-cyanopyridine (0.60 g, 3.43 mmol), triethylamine (0.72 ml, 5.15 mmol) and toluene (100 ml) was refluxed for 48 hrs as described in Example 1. The solvent was concentrated under reduced pressure. The residue was recrystallized from ethanol to give the titled compound (0.30 g, 29%) as crystals.

後処理

  1. temperaturewas refluxed for 48 hrs
  2. concentrationThe solvent was concentrated under reduced pressure
  3. customThe residue was recrystallized from ethanol

出典と根拠

ORDレコード
ord-ad03d1d635a24a25863678d24c54012e
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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