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Sodium Hydroxide → HCID 18455048、化合物

HRID 851983
ノート
印刷プレビュー

反応式

HRID 851983 の反応式
C[O:2][C:3](=[O:30])[C:4]1[CH:9]=[CH:8][C:7]([CH2:10][N:11]([S:20]([C:23]2[CH:28]=[CH:27][C:26]([Cl:29])=[CH:25][CH:24]=2)(=[O:22])=[O:21])[CH:12]2[CH2:18][CH2:17][CH2:16][CH2:15][NH:14][C:13]2=[O:19])=[CH:6][CH:5]=1.[OH-].[Na+]>CO.CC#N>[Cl:29][C:26]1[CH:27]=[CH:28][C:23]([S:20]([N:11]([CH2:10][C:7]2[CH:6]=[CH:5][C:4]([C:3]([OH:30])=[O:2])=[CH:9][CH:8]=2)[CH:12]2[CH2:18][CH2:17][CH2:16][CH2:15][NH:14][C:13]2=[O:19])(=[O:21])=[O:22])=[CH:24][CH:25]=1
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 14798Sodium HydroxideHCID 11568630HCID 11568630、化合物

生成物 1

HCID 18455048HCID 18455048、化合物

試薬・触媒・溶媒 1

HCID 21959252Acetonitrile methanol溶媒

実験手順

rac-4-{[(4-Chloro-benzenesulfonyl)-(2-oxo-azepan-3-yl)-amino]-methyl}-benzoic acid methyl ester (0.95 g, 2.10 mmol) in a mixture of MeOH/CH3CN (50 ml, 1:1 v/v) was treated with 1 N NaOH (2.5 ml) for 24 h. Solvent was removed under reduced pressure and the residue dissolved in ethyl acetate and washed with 5% KHSO4/10% K2SO4 (2×). The aqueous washes were extracted with ethyl acetate and the combined organic fractions were washed with brine, dried (Na2 SO4), filtered, concentrated under reduced pressure and lyophilized from water/CH3CN: lyophilisate, 0.87 g; MS: m/e=435.2 (MH−)

後処理

  1. customSolvent was removed under reduced pressure
  2. dissolutionthe residue dissolved in ethyl acetate
  3. washwashed with 5% KHSO4/10% K2SO4 (2×)
  4. extractionThe aqueous washes were extracted with ethyl acetate
  5. washthe combined organic fractions were washed with brine
  6. customdried (Na2 SO4)
  7. filtrationfiltered
  8. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-004ec35884554f0bb4e74addeaad28d8
出典データセット
uspto-grants-2007_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07253158B2

反応ノート

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