(2,5-Dichlorophenyl)hydrazine → 1-Allyl-2-[(2,5-dichloro-phenyl)-hydrazono]-cyclopentanecarboxylic acid ethyl ester

HRID 1297262ノート

反応式

HRID 1297262 の反応式
[C:1]([C:6]1([CH2:12][CH:13]=[CH2:14])[CH2:10][CH2:9][CH2:8][C:7]1=O)([O:3][CH2:4][CH3:5])=[O:2].[Cl:15][C:16]1[CH:21]=[CH:20][C:19]([Cl:22])=[CH:18][C:17]=1[NH:23][NH2:24].C([O-])(=O)C.[Na+]>CO>[CH2:4]([O:3][C:1]([C:6]1([CH2:12][CH:13]=[CH2:14])[CH2:10][CH2:9][CH2:8][C:7]1=[N:24][NH:23][C:17]1[CH:18]=[C:19]([Cl:22])[CH:20]=[CH:21][C:16]=1[Cl:15])=[O:2])[CH3:5]

参加物

5

反応物 3

HCID 9366(2,5-Dichlorophenyl)hydrazineHCID 517045Sodium AcetateHCID 109104522-Carbethoxy-2-allylcyclopentanone

生成物 1

HCID 866039761-Allyl-2-[(2,5-dichloro-phenyl)-hydrazono]-cyclopentanecarboxylic acid ethyl ester

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a solution of 2-carbethoxy-2-allylcyclopentanone (110 mg, 0.55 mmol) in 1 mL of methanol was added (2,5-dichloro-phenyl)-hydrazine (89 mg, 0.50 mmol) and sodium acetate (62 mg, 0.75 mmol). The reaction mixture was stirred at room temperature over night. The reaction mixture was concentrated and adding 10 mL of ethyl acetate diluted the residue. The organic solution was washed with 5 mL of water and 5 mL of brine. The organic layer was dried over sodium sulfate and concentrated to give the crude product, which was directly used in next step without purification.

後処理

  1. concentrationThe reaction mixture was concentrated
  2. additionadding 10 mL of ethyl acetate
  3. additiondiluted the residue
  4. washThe organic solution was washed with 5 mL of water and 5 mL of brine
  5. dry with materialThe organic layer was dried over sodium sulfate
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-a3e6bf253ea441fda6f8a7a732f98461
出典データセット
uspto-grants-2007_07
特許番号
US07250441B2

反応ノート

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