Malononitrile → HCID 13770581、化合物

HRID 1733146ノート

反応式

HRID 1733146 の反応式
N1CCOCC1.[OH:7][CH2:8][C:9](=O)[C:10]([CH3:13])([CH3:12])[CH3:11].[CH2:15]([C:18]#[N:19])[C:16]#[N:17]>CN(C)C=O>[NH2:19][C:18]1[O:7][CH:8]=[C:9]([C:10]([CH3:13])([CH3:12])[CH3:11])[C:15]=1[C:16]#[N:17]

参加物

5

反応物 3

HCID 8010MalononitrileHCID 8083MorpholineHCID 99558361-Hydroxy-3,3-dimethylbutan-2-one

生成物 1

HCID 13770581HCID 13770581、化合物収率 51.8%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

174 g (2 moles) of morpholine were added dropwise to a solution of 232 g (2 moles) of hydroxy-pinacolone and 132 g (2 moles) of malonic acid dinitrile in 500 ml of dimethylformamide, while cooling, in a manner such that the internal temperature did not rise above 40° C. After the reaction had ended, the reaction mixture was stirred into 5 liters of ice-water. The solid product which thereby precipitated was filtered off, washed with water and dried. 170 g of 2-amino-3-cyano-4-tert.-butyl-furan of melting point 86° C. were obtained in this manner.

後処理

  1. temperaturewhile cooling, in a manner such that the internal temperature
  2. customdid not rise above 40° C
  3. customThe solid product which thereby precipitated
  4. filtrationwas filtered off
  5. washwashed with water
  6. customdried

出典と根拠

ORDレコード
ord-8a7eb99a7da64152ab6244d79dd93ab8
出典データセット
uspto-grants-1980_12
特許番号
US04240820

反応ノート

読み込み中…