Triethylamine → HCID 178510460、化合物

HRID 1715826

反応式

HRID 1715826 の反応式
[N+:1]([C:4]1[CH:15]=[C:8]2[C:9]([O:11][C:12](=O)[NH:13][C:7]2=[CH:6][CH:5]=1)=O)([O-:3])=[O:2].C(#N)C([CH2:19][C:20]#[N:21])O.C([N:25](CC)CC)C>CN(C=O)C>[NH2:25][C:12]1[C:19]([C:20]#[N:21])=[C:9]([OH:11])[C:8]2[C:7](=[CH:6][CH:5]=[C:4]([N+:1]([O-:3])=[O:2])[CH:15]=2)[N:13]=1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 208212H-3,1-Benzoxazine-2,4(1H)-dione, 6-nitro-HCID 212535622-Hydroxybutanedinitrile

生成物 1

HCID 178510460HCID 178510460、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
60 °C

実験手順

To the solution of 47.25 g of 5-nitroisatoic anhydride in 230 mL of DMF 15 g of malonitrile and 63.3 mL of triethylamine were added and the reaction mixture was stirred at 60° C. for 2 hours. The solvent was evaporated at reduced pressure and the residue was mixed with 570 mL of acetonitrile and 114 mL of concd. HCl and the solution was stirred at room temperature overnight. The precipitate was then filtered off, washed with water and ethanol to give 49.7 g of product, m.p.: >360° C. LC-MS: MH+ 231; Ret. time: 4.78 min.

後処理

  1. customThe solvent was evaporated at reduced pressure
  2. additionthe residue was mixed with 570 mL of acetonitrile and 114 mL of concd
  3. stirringHCl and the solution was stirred at room temperature overnight
  4. filtrationThe precipitate was then filtered off
  5. washwashed with water and ethanol

出典と根拠

ORDレコード
ord-41f5f63250a7480cbcf4468c0f181905
出典データセット
uspto-grants-2010_09
特許番号
US07799922B2

関連ノート

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