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Sodium Bicarbonate → HCID 18612735, 화합물

HRID 1180558
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HRID 1180558 반응식
[C:1]([NH:4][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:3])[CH3:2].C(=O)(O)[O-].[Na+]>CO>[C:1]([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:17])=[O:16])[CH:9]([C:10]([O:12][CH3:13])=[O:11])[CH2:14]1)(=[O:3])[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 516892Sodium Bicarbonate2회HCID 18613053HCID 18613053, 화합물

생성물 1

HCID 18612735HCID 18612735, 화합물수율 79.1%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

To a solution of methyl 2-[(2-acetylamino-benzyl)-(4-methoxybenzenesulfonyl)amino]acrylate (8.40 g, 20.07 mmol) in anhydrous methanol (5 ml) was added anhydrous sodium bicarbonate (2.19 g, 26.09 mmol) and the mixture was stirred at room temperature overnight. Anhydrous sodium bicarbonate (2.2 g) was added and the mixture was stirred for 18 hours, heated to 50° C. for three hours and the solvent removed in vacuo. The residue was dissolved in water and ethyl acetate. The organic layer was separated, washed with saturated sodium chloride and dried with anhydrous sodium sulfate. The solvent was removed in vacuo and the residue dried in vacuo to give 6.64 g of white crystals, m.p. 150-155° C.

후처리

  1. stirringthe mixture was stirred for 18 hours
  2. temperatureheated to 50° C. for three hours
  3. customthe solvent removed in vacuo
  4. dissolutionThe residue was dissolved in water
  5. customThe organic layer was separated
  6. washwashed with saturated sodium chloride
  7. dry with materialdried with anhydrous sodium sulfate
  8. customThe solvent was removed in vacuo
  9. customthe residue dried in vacuo

출처 및 근거

ORD 기록
ord-21acd2bac17f42238b98403f49c5fd1b
출처 데이터셋
uspto-grants-2007_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07282496B2

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