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Sodium Hydroxide → HCID 18455048, 화합물

HRID 851983
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HRID 851983 반응식
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
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참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 11568630HCID 11568630, 화합물

생성물 1

HCID 18455048HCID 18455048, 화합물

시약·촉매·용매 1

HCID 21959252Acetonitrile methanol용매

실험 절차

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−)

후처리

  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

출처 및 근거

ORD 기록
ord-004ec35884554f0bb4e74addeaad28d8
출처 데이터셋
uspto-grants-2007_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07253158B2

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