Triethylamine → HCID 178517389、化合物

HRID 23906

反応式

HRID 23906 の反応式
[F:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[C:4]([F:9])[C:3]=1[CH:10]([C:16]([O:18]CC)=O)[C:11](OCC)=[O:12].C(N(CC)CC)C.[NH2:28][C:29]1[N:33]=[CH:32][NH:31][N:30]=1.[OH-].[Na+]>O>[OH:18][C:16]1[C:10]([C:3]2[C:2]([F:1])=[CH:7][C:6]([F:8])=[CH:5][C:4]=2[F:9])=[C:11]([OH:12])[N:30]2[N:31]=[CH:32][N:33]=[C:29]2[N:28]=1

参加物

6

反応物 4

HCID 8471TriethylamineHCID 14798Sodium HydroxideHCID 2782662Propanedioic acid, 2-(2,4,6-trifluorophenyl)-, 1,3-diethyl esterHCID 178418311HCID 178418311、化合物

生成物 1

HCID 178517389HCID 178517389、化合物

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 22 mmol of diethyl 2-(2,4,6-trifluorophenyl)malonate, 24 mmol of triethylamine and 22 mmol of 3-amino-1,2,4-triazole was heated with stirring at 180° C. for 6 hours. The reaction mixture was then cooled to 50° C., admixed with a solution of 2.2 g of sodium hydroxide in 25 ml of water and stirred for 30 minutes. The aqueous phase was washed with ether and then acidified with conc. hydrochloric acid. The precipitated colorless solid was filtered off, washed with water and diisopropyl ether and dried. The yield of the title compound was 85% (m.p.: 200-201° C.).

後処理

  1. temperaturewas heated
  2. temperatureThe reaction mixture was then cooled to 50° C.
  3. stirringstirred for 30 minutes
  4. washThe aqueous phase was washed with ether
  5. filtrationThe precipitated colorless solid was filtered off
  6. washwashed with water and diisopropyl ether
  7. customdried

出典と根拠

ORDレコード
ord-44d9929e86744a49a72323548ff6e76e
出典データセット
uspto-grants-2005_02
特許番号
US06855718B2

関連ノート

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