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Sodium Bicarbonate → HCID 18612735、化合物

HRID 1180558
ノート
印刷プレビュー

反応式

HRID 1180558 の反応式
[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]
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 516892Sodium Bicarbonate2 回HCID 18613053HCID 18613053、化合物

生成物 1

HCID 18612735HCID 18612735、化合物収率 79.1%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-21acd2bac17f42238b98403f49c5fd1b
出典データセット
uspto-grants-2007_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07282496B2

反応ノート

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