Sodium Acetate → Ethyl 2-chloro-5-(3,3,3-trifluoro-2-oxopropylidenehydrazino)cinnamate

HRID 48496

反応式

HRID 48496 の反応式
C([O-])(=O)C.[Na+].Br[CH:7](Br)[C:8]([C:10]([F:13])([F:12])[F:11])=[O:9].[Cl:15][C:16]1[CH:28]=[CH:27][C:26]([NH:29][NH2:30])=[CH:25][C:17]=1[CH:18]=[CH:19][C:20]([O:22][CH2:23][CH3:24])=[O:21]>O>[Cl:15][C:16]1[CH:28]=[CH:27][C:26]([NH:29][N:30]=[CH:7][C:8](=[O:9])[C:10]([F:13])([F:12])[F:11])=[CH:25][C:17]=1[CH:18]=[CH:19][C:20]([O:22][CH2:23][CH3:24])=[O:21]

参加物

5

反応物 3

HCID 517045Sodium AcetateHCID 5505231,1-Dibromo-3,3,3-trifluoroacetoneHCID 54155293Ethyl 2-chloro-5-hydrazinocinnamate

生成物 1

HCID 69141416Ethyl 2-chloro-5-(3,3,3-trifluoro-2-oxopropylidenehydrazino)cinnamate収率 97.5%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
80 °C

実験手順

First, 7.4 g (90.2 mmol) of sodium acetate and 8.0 g (28.2 mmol) of 1,1-dibromo-3,3,3-trifluoroacetone were mixed with 70 ml of water, and the mixture was stirred at 80° C. for 30 minutes and then cooled, to which 7.0 g of ethyl 2-chloro-5-hydrazinocinnamate was added at 10° C. or lower, and the mixture was stirred for 3 hours. The precipitated crystals were collected by filtration and dried, which afforded 9.6 g (27.5 mmol) of ethyl 2-chloro-5-(3,3,3-trifluoro-2-oxopropylidenehydrazino)cinnamate.

後処理

  1. additionwas added at 10° C.
  2. stirringlower, and the mixture was stirred for 3 hours
  3. filtrationThe precipitated crystals were collected by filtration
  4. customdried

出典と根拠

ORDレコード
ord-f6842c74bf1f4c02a4882ecb818c07ca
出典データセット
uspto-grants-2004_03
特許番号
US06703503B2

関連ノート

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