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Sodium Hydroxide → HCID 136209541、化合物

HRID 1195459
ノート
印刷プレビュー

反応式

HRID 1195459 の反応式
Cl.[CH2:2]([O:4][NH2:5])[CH3:3].[OH-].[Na+].[OH:8][C:9]1[CH2:14][CH:13]([C:15]2[CH:16]=[C:17]3[C:21](=[CH:22][CH:23]=2)[CH2:20][CH2:19][CH2:18]3)[CH2:12][C:11](=[O:24])[C:10]=1[C:25](=O)[CH2:26][CH3:27]>C(O)C>[CH2:2]([O:4][N:5]=[C:25]([C:10]1[C:9](=[O:8])[CH2:14][CH:13]([C:15]2[CH:16]=[C:17]3[C:21](=[CH:22][CH:23]=2)[CH2:20][CH2:19][CH2:18]3)[CH2:12][C:11]=1[OH:24])[CH2:26][CH3:27])[CH3:3]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 14798Sodium HydroxideHCID 76850O-ethylhydroxylamine hydrochlorideHCID 178458818HCID 178458818、化合物

生成物 1

HCID 136209541HCID 136209541、化合物収率 94.8%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

Ethoxyamine hydrochloride (0.42 g; 4.1 mmole) and then aqueous 1% sodium hydroxide (17.0 ml) were added to a solution of 3-hydroxy-5-(5-indanyl)-2-propionylcyclohex-2-en-one (1.10 g; 3.87 mmole) in anhydrous absolute ethanol (200 ml). The mixture was stirred at room temperature for a period of 4 hours and then the ethanol was removed by evaporation under reduced pressure using a rotary evaporator. The residue was treated with dichloromethane and the organic phase was washed twice with dilute aqueous hydrochloric acid and twice with water. The organic phase was dried over anhydrous sodium sulphate and the solvent was removed by evaporation under reduced pressure to give the product, 2-[1-(ethoxyimino)propyl]-3-hydroxy-5-(5-indanyl)-cyclohex-2-en-1-one (1.20 g; 94.8%) as a pale yellow oil.

後処理

  1. customthe ethanol was removed by evaporation under reduced pressure
  2. customa rotary evaporator
  3. additionThe residue was treated with dichloromethane
  4. washthe organic phase was washed twice with dilute aqueous hydrochloric acid and twice with water
  5. dry with materialThe organic phase was dried over anhydrous sodium sulphate
  6. customthe solvent was removed by evaporation under reduced pressure

出典と根拠

ORDレコード
ord-cf448421042b44b3b0a23f1cfa3fb3a7
出典データセット
uspto-grants-1992_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05110989

反応ノート

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