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Lithium Hydroxide → HCID 66756006、化合物

HRID 1642140
ノート
印刷プレビュー

反応式

HRID 1642140 の反応式
[OH-].[Li+].[Cl:3][C:4]1[CH:9]=[C:8]([Cl:10])[CH:7]=[CH:6][C:5]=1[S:11]([N:14]1[CH2:19][CH2:18][NH:17][C:16](=[O:20])[CH:15]1[CH2:21][C:22]([O:24]CC)=[O:23])(=[O:13])=[O:12]>CO.O>[Cl:3][C:4]1[CH:9]=[C:8]([Cl:10])[CH:7]=[CH:6][C:5]=1[S:11]([N:14]1[CH2:19][CH2:18][NH:17][C:16](=[O:20])[CH:15]1[CH2:21][C:22]([OH:24])=[O:23])(=[O:13])=[O:12]
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 2

HCID 3939Lithium HydroxideHCID 3767271Ethyl 2-{1-[(2,4-dichlorophenyl)sulfonyl]-3-oxo-2-piperazinyl}acetate

生成物 1

HCID 66756006HCID 66756006、化合物

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒

実験手順

Lithium hydroxide (0.92 mg, 21.9 mmol) was added to a cooled solution of ethyl 2-(1-(2,4-dichlorophenylsulfonyl)-3-oxopiperazin-2-yl)acetate (2.7 g, 7.3 mmol) in methanol (25 ml) and water (6 ml), and stirring was carried out for 16 h at room temperature (TLC monitoring). The solvent was removed using a rotary evaporator and the residue was taken up in water. The aqueous phase was washed with diethyl ether and acidified with HCl, and the product was extracted with ethyl acetate. The organic phase was then washed with saturated NaCl solution. The organic phase was dried over sodium sulfate and concentrated to dryness.

後処理

  1. customThe solvent was removed
  2. customa rotary evaporator
  3. washThe aqueous phase was washed with diethyl ether
  4. extractionthe product was extracted with ethyl acetate
  5. washThe organic phase was then washed with saturated NaCl solution
  6. dry with materialThe organic phase was dried over sodium sulfate
  7. concentrationconcentrated to dryness

出典と根拠

ORDレコード
ord-a830e8ac4c3b472a91f642206594d231
出典データセット
uspto-grants-2012_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08119633B2

反応ノート

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