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Tributylamine → HCID 178509618、化合物

HRID 857926
ノート
印刷プレビュー

反応式

HRID 857926 の反応式
[NH2:1][C:2]1[N:6]=[CH:5][NH:4][N:3]=1.[C:7]([C:9]1[CH:14]=[CH:13][C:12]([CH:15]([C:21](OCC)=[O:22])[C:16](OCC)=[O:17])=[CH:11][CH:10]=1)#[N:8].C(N(CCCC)CCCC)CCC.[OH-].[Na+]>O>[OH:17][C:16]1[C:15]([C:12]2[CH:13]=[CH:14][C:9]([C:7]#[N:8])=[CH:10][CH:11]=2)=[C:21]([OH:22])[N:3]2[N:4]=[CH:5][N:6]=[C:2]2[N:1]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 7622TributylamineHCID 14798Sodium HydroxideHCID 11737076Diethyl (4-cyanophenyl)propanedioateHCID 178418311HCID 178418311、化合物

生成物 1

HCID 178509618HCID 178509618、化合物収率 66.4%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
180 °C

実験手順

A mixture of 14 g of 3-amino-1,2,4-triazole, 0.17 mol of the ester from example 1 and 50 ml of tributylamine (50 ml) was stirred at 180° C. for approximately 6 hours. A solution of 21 g of NaOH in 200 ml of water was added at approximately 700 and the mixture was stirred for a further 30 min. The organic phase was separated and the aqueous phase was extracted with diethyl ether. The product precipitated from the aqueous phase after acidification with concentrated hydrochloric acid. 28 g of the title compound were obtained by filtration.

後処理

  1. stirringthe mixture was stirred for a further 30 min
  2. customThe organic phase was separated
  3. extractionthe aqueous phase was extracted with diethyl ether
  4. customThe product precipitated from the aqueous phase after acidification with concentrated hydrochloric acid

出典と根拠

ORDレコード
ord-35e276461e314910b85204b5b4f94f03
出典データセット
uspto-grants-2006_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07148227B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート