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Potassium Carbonate → HCID 13853901、化合物

HRID 2372351
ノート
印刷プレビュー

反応式

HRID 2372351 の反応式
Cl.[CH2:2]([O:4][C:5]1[CH:12]=[CH:11][C:8]([CH2:9][NH2:10])=[CH:7][CH:6]=1)[CH3:3].[Br:13][C:14]1[C:15](=[O:24])[N:16]([CH:21]([CH3:23])[CH3:22])[N:17]=[CH:18][C:19]=1Br.C(=O)([O-])[O-].[K+].[K+].O1CCOCC1>O>[Br:13][C:14]1[C:15](=[O:24])[N:16]([CH:21]([CH3:22])[CH3:23])[N:17]=[CH:18][C:19]=1[NH:10][CH2:9][C:8]1[CH:11]=[CH:12][C:5]([O:4][CH2:2][CH3:3])=[CH:6][CH:7]=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 11430Potassium CarbonateHCID 312751,4-DioxaneHCID 10827742HCID 10827742、化合物HCID 18975845HCID 18975845、化合物

生成物 1

HCID 13853901HCID 13853901、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
90 °C

実験手順

A mixture of 0.38 g of 4-ethoxybenzylamine hydrochloride, 0.4 g of 4,5-dibromo-2-iso-propyl-3(2H)pyridazinone, 0.34 g of potassium carbonate, 6 ml of 1,4-dioxane and 18 ml of water, was heated at 90° C. under stirring for 10 hours. The sovent was distilled off under reduced pressure, and water was added to the residue thereby obtained, and the mixture was extracted with ethyl acetate. The extract was washed with diluted hydrochloric acid and a saturated sodium chloride aqueous solution, and dried over sodium sulfate, and then the solvent was distilled off. The product was crystallized from ether to obtain 220 mg of the above identified compound having a melting point of from 151° to 152.5° C. as pale yellow crystals.

後処理

  1. distillationThe sovent was distilled off under reduced pressure, and water
  2. additionwas added to the residue
  3. customthereby obtained
  4. extractionthe mixture was extracted with ethyl acetate
  5. washThe extract was washed with diluted hydrochloric acid
  6. dry with materiala saturated sodium chloride aqueous solution, and dried over sodium sulfate
  7. distillationthe solvent was distilled off
  8. customThe product was crystallized from ether
  9. customto obtain 220 mg of the
  10. customof from 151° to 152.5° C.

出典と根拠

ORDレコード
ord-9c2b6825c3434f8c941796b2eae9f43d
出典データセット
uspto-grants-1992_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05098900

反応ノート

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