5-Chloro-2-furaldehyde → 1-(5-Chloro-furfurylidene-amino)-2,3-dioxo-piperazine

HRID 2051764

反応式

HRID 2051764 の反応式
[Cl:1][C:2]1[O:8][C:5]([CH:6]=O)=[CH:4][CH:3]=1.[NH2:9][N:10]1[CH2:15][CH2:14][NH:13][C:12](=[O:16])[C:11]1=[O:17]>C(O)(=O)C>[Cl:1][C:2]1[O:8][C:5]([CH:6]=[N:9][N:10]2[CH2:15][CH2:14][NH:13][C:12](=[O:16])[C:11]2=[O:17])=[CH:4][CH:3]=1

参加物

4

反応物 2

HCID 27696305-Chloro-2-furaldehydeHCID 221847681-Aminopiperazine-2,3-dione

生成物 1

HCID 540375391-(5-Chloro-furfurylidene-amino)-2,3-dioxo-piperazine収率 74.6%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

1.6 pts. by wt. of 5-chloro-furfural, 1.3 pts. by wt. of 1-amino-2,3-dioxo-piperazine and 7 pts. by vol. of glacial acetic acid are warmed to 90° C. for 10 minutes and then left for 30 minutes at RT. The precipitate is filtered off, washed first with 3 pts. by vol. of glacial acetic acid and then twice with 10 pts. by vol. of acetonitrile each time and dried in air. 1.8 pts. by wt. (74.6%) of 1-(5-chloro-furfurylidene-amino)-2,3-dioxo-piperazine are obtained as yellowish crystals of decomp. pt. 233°-6° C.

後処理

  1. filtrationThe precipitate is filtered off
  2. washwashed first with 3 pts
  3. dry with materialby vol. of acetonitrile each time and dried in air

出典と根拠

ORDレコード
ord-dd26e4d2762f451a9ea948170f20d677
出典データセット
uspto-grants-1980_01
特許番号
US04182762

関連ノート

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