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Sodium Bicarbonate → HCID 18612735, 화합물

HRID 1264587
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HRID 1264587 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.

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-bdf1882e369a48199614b9856e4957f5
출처 데이터셋
uspto-grants-2003_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06544984B1

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