Potassium Hydroxide → 2,3,4,5-Tetrahydro-1,4-benzoxazepin-5-one

HRID 1946632

反応式

HRID 1946632 の反応式
[O:1]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[C:4](=[O:11])[CH2:3][CH2:2]1.[N-:12]=[N+]=[N-].[Na+].[OH-].[K+]>S(=O)(=O)(O)O>[O:1]1[C:10]2[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=2[C:4](=[O:11])[NH:12][CH2:3][CH2:2]1

参加物

5

反応物 3

HCID 14797Potassium HydroxideHCID 33557Sodium AzideHCID 68110Chromanone

生成物 1

HCID 3406292,3,4,5-Tetrahydro-1,4-benzoxazepin-5-one

試薬・触媒・溶媒 1

HCID 1118Sulfuric Acid溶媒2 回

実験手順

The chroman-4-one (5.0 g, 33.8 mmol) was dissolved in sulfuric acid (10 mL) and the mixture was cooled at 0 oC. Sodium azide (2.88 g, 44.3 mmol) was added portionwise followed by some sulfuric acid (5 mL). The reaction mixture was stirred at room temperature over night. The mixture was then pour into ice-water and basified to pH=7 with potassium hydroxide pellets. This aqueous layer was extracted with ether (twice).

後処理

  1. temperaturethe mixture was cooled at 0 oC
  2. extractionThis aqueous layer was extracted with ether (twice)

出典と根拠

ORDレコード
ord-88a9b647d76b4d0aa3e7a773eadd29f4
出典データセット
uspto-grants-2013_03
特許番号
US08399452B2

関連ノート

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