Iodoethane → Ethyl 2-isonicotinoylthiophene-3-carboxylate

HRID 1498885ノート

反応式

HRID 1498885 の反応式
[C:1]([C:9]1[S:10][CH:11]=[CH:12][C:13]=1[C:14]([OH:16])=[O:15])(=[O:8])[C:2]1[CH:7]=[CH:6][N:5]=[CH:4][CH:3]=1.C([O-])([O-])=O.[Cs+].[Cs+].[CH3:23][CH2:24]I>CC#N>[C:1]([C:9]1[S:10][CH:11]=[CH:12][C:13]=1[C:14]([O:16][CH2:23][CH3:24])=[O:15])(=[O:8])[C:2]1[CH:7]=[CH:6][N:5]=[CH:4][CH:3]=1

参加物

5

反応物 3

HCID 6340IodoethaneHCID 10796Cesium carbonateHCID 866831162-Isonicotinoylthiophene-3-carboxylic acid

生成物 1

HCID 86683117Ethyl 2-isonicotinoylthiophene-3-carboxylate収率 85.5%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

反応条件

温度
30 °C

実験手順

To a solution of 2-isonicotinoylthiophene-3-carboxylic acid (2.2 g, 9.4 mmol) from example 2.1 and Cs2CO3 (6.2 g, 18.9 mmol) in CH3CN (500 mL) was added CH3CH2I (2.9 g, 18.9 mmol) dropwise. The mixture was stirred at 30° C. for 48 h. The mixture was filtered and concentrated to give the title compound (2.1 g, 85.5% yield) as yellow oil. LC-MS (Method A): m/z 340 (M+H)+, Rt: 0.81 min.

後処理

  1. filtrationThe mixture was filtered
  2. concentrationconcentrated

出典と根拠

ORDレコード
ord-b52c70d465e6462fb1f79944b0275241
出典データセット
uspto-grants-2015_12
特許番号
US09200005B2

反応ノート

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