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Sodium Hydroxide → HCID 19853902、化合物

HRID 1723062
ノート
印刷プレビュー

反応式

HRID 1723062 の反応式
[CH3:1][C:2]1([CH3:21])[CH2:8][CH2:7][CH2:6][C:5]2[C:9]([NH:17]C(=O)C)=[CH:10][CH:11]=[C:12]([C:13]([O:15]C)=[O:14])[C:4]=2[O:3]1.[OH-].[Na+]>CO>[CH3:1][C:2]1([CH3:21])[CH2:8][CH2:7][CH2:6][C:5]2[C:9]([NH2:17])=[CH:10][CH:11]=[C:12]([C:13]([OH:15])=[O:14])[C:4]=2[O: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 19853911HCID 19853911、化合物

生成物 1

HCID 19853902HCID 19853902、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a solution of 5.5 g (19.0 mmol) of methyl 2,2-dimethyl-6-acetylamino-2,3,4,5-tetrahydro-1-benzoxepin-9-carboxylate in 10 ml of methanol is added 10 ml of a 10% aqueous sodium hydroxide solution in a single portion at room temperature. The reaction mixture is heated to reflux and maintained at that temperature for 2 hours. After cooling, methanol is removed in vacuo and the residue is diluted with water. The pH of the solution is adjusted to 7 with 1N HCl and the solution is extracted with CH2Cl2. The combined organic extracts are dried over MgSO4, filtered and concentrated. Flash chromatography (30% EtOAc/hexanes) gives 2,2-dimethyl-6-amino-2,3,4,5-tetrahydro-1-benzoxepin-9-carboxylic acid.

後処理

  1. temperatureThe reaction mixture is heated
  2. temperatureto reflux
  3. temperaturemaintained at that temperature for 2 hours
  4. temperatureAfter cooling
  5. custommethanol is removed in vacuo
  6. additionthe residue is diluted with water
  7. extractionthe solution is extracted with CH2Cl2
  8. dry with materialThe combined organic extracts are dried over MgSO4
  9. filtrationfiltered
  10. concentrationconcentrated

出典と根拠

ORDレコード
ord-8eef148c44d645eeb13ab02b954119da
出典データセット
uspto-grants-1989_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04859683

反応ノート

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