Tributylamine → HCID 178517388、化合物

HRID 2357872ノート

反応式

HRID 2357872 の反応式
[NH2:1][C:2]1[N:6]=[CH:5][NH:4][N:3]=1.C([O:9][C:10](=O)[CH:11]([C:17]1[CH:22]=[C:21]([F:23])[CH:20]=[C:19]([F:24])[C:18]=1[F:25])[C:12](OCC)=[O:13])C.C(N(CCCC)CCCC)CCC>[OH-].[Na+]>[OH:9][C:10]1[C:11]([C:17]2[CH:22]=[C:21]([F:23])[CH:20]=[C:19]([F:24])[C:18]=2[F:25])=[C:12]([OH:13])[N:3]2[N:4]=[CH:5][N:6]=[C:2]2[N:1]=1

参加物

5

反応物 3

HCID 7622TributylamineHCID 68637486HCID 68637486、化合物HCID 178418311HCID 178418311、化合物

生成物 1

HCID 178517388HCID 178517388、化合物収率 91.5%

試薬・触媒・溶媒 1

HCID 14798Sodium Hydroxide溶媒

反応条件

温度
180 °C

実験手順

A mixture of 3-amino-1,2,4-triazole (14 g), diethyl(2,3,5-trifluorophenyl)-malonate (0.17 mol, obtained from Ex. 1) and tributylamine (50 ml) was heated at 180° C. for six hours. The reaction mixture was cooled to about 70° C. After addition of aqueous sodium hydroxide (21 g/200 ml H2O) the reaction mixture was stirred for 30 minutes. After separation of the organic phase the aqueous phase was extracted with diethyl ether. The aqueous phase was acidified with concentrated hydrochloric acid. The precipitate was collected by filtration and dried to yield 43 g of the title compound.

後処理

  1. temperatureThe reaction mixture was cooled to about 70° C
  2. customAfter separation of the organic phase the aqueous phase
  3. extractionwas extracted with diethyl ether
  4. filtrationThe precipitate was collected by filtration
  5. customdried

出典と根拠

ORDレコード
ord-188ccdc085d6488c9d5f450cebfd9730
出典データセット
uspto-grants-2010_07
特許番号
US07763622B2

反応ノート

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