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Sodium Hydroxide → 2-[[(8-chlorodibenz[b,f][1,4]oxazepin-10(11H)-yl)carbonyl]amino]acetic acid

HRID 1756537
ノート
印刷プレビュー

反応式

HRID 1756537 の反応式
[Cl:1][C:2]1[CH:25]=[CH:24][C:5]2[O:6][C:7]3[CH:23]=[CH:22][CH:21]=[CH:20][C:8]=3[CH2:9][N:10]([C:11]([NH:13][CH2:14][C:15]([O:17]CC)=[O:16])=[O:12])[C:4]=2[CH:3]=1.[OH-].[Na+]>CO>[Cl:1][C:2]1[CH:25]=[CH:24][C:5]2[O:6][C:7]3[CH:23]=[CH:22][CH:21]=[CH:20][C:8]=3[CH2:9][N:10]([C:11]([NH:13][CH2:14][C:15]([OH:17])=[O:16])=[O:12])[C:4]=2[CH:3]=1
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 14798Sodium HydroxideHCID 10570547HCID 10570547、化合物

生成物 1

HCID 108304472-[[(8-chlorodibenz[b,f][1,4]oxazepin-10(11H)-yl)carbonyl]amino]acetic acid収率 99.5%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To the product of Example 3 (5.1 g, 14.2 mmol) dissolved in 100 mL of methanol (MeOH) was added 25 mL (25.0 mmol) of 1N sodium hydroxide (NaOH). This reaction was stirred at room temperature overnight before all solvent was removed under reduced pressure. The residue was dissolved in 250 mL of water and the solution was brought to pH 3 with 1N HCl. The product was extracted from the aqueous phase with 3×250 mL of Et2O. The Et2O layer was then dried (Na2SO4), filtered, and stripped of all solvent under reduced pressure to provide 4.7 g of the title compound after drying in a vacuum oven.

後処理

  1. customwas removed under reduced pressure
  2. dissolutionThe residue was dissolved in 250 mL of water
  3. extractionThe product was extracted from the aqueous phase with 3×250 mL of Et2O
  4. dry with materialThe Et2O layer was then dried (Na2SO4)
  5. filtrationfiltered

出典と根拠

ORDレコード
ord-b4a352933bee4c47a0b9bf208f423507
出典データセット
uspto-grants-1995_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05441950

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート