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Sodium Bicarbonate → HCID 18612735, 화합물

HRID 1420596
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HRID 1420596 반응식
C([N:4]([C:30](=[O:32])[CH3:31])[C:5]1[CH:29]=[CH:28][CH:27]=[CH:26][C:6]=1[CH2:7][N:8]([S:15]([C:18]1[CH:23]=[CH:22][C:21]([O:24][CH3:25])=[CH:20][CH:19]=1)(=[O:17])=[O:16])[C:9](=[CH2:14])[C:10]([O:12][CH3:13])=[O:11])(=O)C.C(=O)(O)[O-].[Na+]>CO>[C:30]([N:4]1[C:5]2[CH:29]=[CH:28][CH:27]=[CH:26][C:6]=2[CH2:7][N:8]([S:15]([C:18]2[CH:19]=[CH:20][C:21]([O:24][CH3:25])=[CH:22][CH:23]=2)(=[O:16])=[O:17])[CH:9]([C:10]([O:12][CH3:13])=[O:11])[CH2:14]1)(=[O:32])[CH3:31]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 516892Sodium BicarbonateHCID 18612823Methyl 2-[(2-diacetylaminobenzyl)-(4-methoxybenzenesulfonyl)amino]acrylate

생성물 1

HCID 18612735HCID 18612735, 화합물수율 92.8%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

To a solution of 0.70 g (1.52 mmol) of methyl 2-[(2-diacetylaminobenzyl)-(4-methoxybenzenesulfonyl)amino]acrylate in 5 ml of anhydrous methanol was added 0.332 g (3.95 mmol) of anhydrous sodium bicarbonate. The mixture was stirred at room temperature overnight and the solvent removed under vacuum. To the residue was added ethyl acetate and H2O. The organic layer was separated, washed with brine and dried with Na2SO4. The solvent was removed and the residue dried under vacuum to give 0.59 g of white crystals, m.p. 150-155° C. Anal. for C20H22N2O6S: Calc'd: C,57.4; H,5.3; N,6.7; S,7.7; Found: C,56.6; H,5.2; N,6.5; S,7.5; Mass spectrum (ES) 419.9 (M+H).

후처리

  1. customthe solvent removed under vacuum
  2. additionTo the residue was added ethyl acetate and H2O
  3. customThe organic layer was separated
  4. washwashed with brine
  5. dry with materialdried with Na2SO4
  6. customThe solvent was removed
  7. customthe residue dried under vacuum

출처 및 근거

ORD 기록
ord-67b772de02604e81a1bef3fd27f29ba5
출처 데이터셋
uspto-grants-2000_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06071903

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