Magnesium orthosilicate → 2-Cyano-3dimethylamino-1-thien-3-ylpropen-1-one

HRID 345968ノート

反応式

HRID 345968 の反応式
[S:1]1[CH:5]=[CH:4][C:3]([C:6]2[O:10][N:9]=[CH:8][CH:7]=2)=[CH:2]1.CO[CH:13](OC)[N:14]([CH3:16])[CH3:15].[Si]([O-])([O-])([O-])[O-].[Mg+2].[Mg+2]>C(Cl)Cl>[CH3:16][N:14]([CH:13]=[C:7]([C:6](=[O:10])[C:3]1[CH:4]=[CH:5][S:1][CH:2]=1)[C:8]#[N:9])[CH3:15]

参加物

5

反応物 3

HCID 66225Magnesium orthosilicateHCID 78373Dimethylformamide dimethyl acetalHCID 185168865-(Thiophen-3-yl)isoxazole

生成物 1

HCID 299434852-Cyano-3dimethylamino-1-thien-3-ylpropen-1-one収率 56.5%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A mixture of 41.2 g of 5-(3-thienyl)isoxazole and 36.0 g of dimethylformamide dimethylacetal, under nitrogen, is heated on a stream bath for 4 hours. The reaction is concentrated in vacuo to give a viscous oil which solidified. The residue is dissolved in methylene chloride and passed thru a short column of hydrous magnesium silicate. On cooling, 31.76 g of the desired product is obtained, mp 118°-119°, CI-MS:m/z 206(M30). Concentrating in vacuo the methylene chloride gives an additional 20.2 g of product. (Total recovered 51.96 g, 92%).

後処理

  1. temperatureunder nitrogen, is heated on a stream bath for 4 hours
  2. concentrationThe reaction is concentrated in vacuo
  3. customto give a viscous oil which
  4. temperatureOn cooling

出典と根拠

ORDレコード
ord-c173186a7e67482f8013b66cca805112
出典データセット
uspto-grants-1991_10
特許番号
US05059709

反応ノート

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