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Hydrochloric Acid → HCID 20164696、化合物

HRID 255840
ノート
印刷プレビュー

反応式

HRID 255840 の反応式
C([O:3][C:4]([C:6]([CH:14]([CH2:23][C:24]#[CH:25])[C:15]1[CH:20]=[CH:19][C:18]([Cl:21])=[CH:17][C:16]=1[Cl:22])([C:8]1[CH:9]=[N:10][CH:11]=[CH:12][CH:13]=1)[OH:7])=[CH2:5])C.Cl>CO>[Cl:22][C:16]1[CH:17]=[C:18]([Cl:21])[CH:19]=[CH:20][C:15]=1[CH:14]([CH2:23][C:24]#[CH:25])[C:6]([OH:7])([C:8]1[CH:9]=[N:10][CH:11]=[CH:12][CH:13]=1)[C:4](=[O:3])[CH3:5]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 20164645HCID 20164645、化合物

生成物 1

HCID 20164696HCID 20164696、化合物収率 97.3%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A mixture of 2.0 g of α-(1-ethoxyvinyl)-α-[2,4-dichloro-α-(2-propynyl)-benzyl]-3-pyridinemethanol (see Example 3, 1st end product), 1 ml of concentrated hydrochloric acid and 15 ml of methanol as a clear yellow solution is held at room temperature for 1 hour. Thereafter, the mixture is evaporated under reduced pressure in order to remove methanol and the residue is neutralized with saturated aqueous sodium bicarbonate solution. The aqueous mixture is extracted with ethyl acetate and the organic phase is washed with saturated aqueous sodium chloride solution and evaporated. Finally, the residue is recrystallized from methylene chloride/n-hexane. There are obtained 1.8 g of 4-(2,4-dichlorophenyl)-3-hydroxy-3-(3-pyridyl)-6-heptyn-2-one, m.p. 132° C.

後処理

  1. customThereafter, the mixture is evaporated under reduced pressure in order
  2. customto remove methanol
  3. extractionThe aqueous mixture is extracted with ethyl acetate
  4. washthe organic phase is washed with saturated aqueous sodium chloride solution
  5. customevaporated
  6. customFinally, the residue is recrystallized from methylene chloride/n-hexane

出典と根拠

ORDレコード
ord-f4efa9d6aa6846789db741a00ed5ed54
出典データセット
uspto-grants-1987_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04699652

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート