Methanol → HCID 178471968、化合物

HRID 240312

反応式

HRID 240312 の反応式
[CH2:1]([O:3][C:4](=[O:8])[CH2:5][C:6]#[N:7])[CH3:2].[H-].[Na+].[O:11]=[C:12]1[C:24]2[C:19](=[N:20][C:21](C#N)=[C:22]([C:25]#[N:26])[N:23]=2)[C:18]2[CH:17]=[CH:16][CH:15]=[CH:14][C:13]1=2.CO>CN(C=O)C>[C:6]([C:5]([C:21]1[N:20]=[C:19]2[C:18]3[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=3[C:12](=[O:11])[C:24]2=[N:23][C:22]=1[C:25]#[N:26])=[C:4]([O:3][CH2:1][CH3:2])[OH:8])#[N:7]

参加物

6

反応物 4

HCID 887MethanolHCID 7764Ethyl cyanoacetateHCID 24758Sodium hydrideHCID 2929299-oxo-9H-indeno(1,2-b)pyrazine-2,3-dicarbonitrile

生成物 1

HCID 178471968HCID 178471968、化合物収率 97.3%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

実験手順

Ethylcyanoacetate (110 mg, 0.970 mmol) was dissolved, under inert atmosphere, in dry DMF (1 ml) and NaH (39 mg, 0.970 mmol) was added in one portion. After 30 min, a solution of 1 (150 mg, 0.646 mmol) in dry DMF (2 ml) was added dropwise. After 15 min MeOH was added and the solution stirred for 10 min. The solvents were evaporated and the crude purified by flash chromatography (EtOAc:MeOH 9:1) affording 22 as a dark red solid (200 mg, 97%).

後処理

  1. customThe solvents were evaporated
  2. customthe crude purified by flash chromatography (EtOAc:MeOH 9:1)

出典と根拠

ORDレコード
ord-acdda630ff26422c8d67586bdcbc4117
出典データセット
uspto-grants-2014_02
特許番号
US08648076B2

関連ノート

読み込み中…