Hydroxyamine hydrochloride → N-[(1S)-1,3,3-Trimethylbicyclo[2.2.1]heptan-2-ylidene]hydroxylamine

HRID 582917ノート

反応式

HRID 582917 の反応式
Cl.[NH2:2][OH:3].C([O-])(=O)C.[Na+].[CH3:9][C@@:10]12[C:16](=O)[C:15]([CH3:19])([CH3:18])[C@@H:13]([CH2:14]1)[CH2:12][CH2:11]2>O.CO>[CH3:9][C@@:10]12[CH2:14][CH:13]([CH2:12][CH2:11]1)[C:15]([CH3:19])([CH3:18])[C:16]2=[N:2][OH:3]

参加物

6

反応物 3

HCID 443297Hydroxyamine hydrochlorideHCID 517045Sodium AcetateHCID 1201521d-Fenchone

生成物 1

HCID 71362104N-[(1S)-1,3,3-Trimethylbicyclo[2.2.1]heptan-2-ylidene]hydroxylamine収率 98%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒

実験手順

A solution of 23 g of hydroxylamine hydrochloride and 41 g of sodium acetate in 200 ml of water is added at RT to a solution of 38.1 g of (1S)-(+)-fenchone in 120 ml of MeOH and the mixture is then refluxed for 48 hours. After cooling to RT, the precipitate formed is filtered off, washed with water and dried under vacuum to give 41 g of the expected product.

後処理

  1. temperaturethe mixture is then refluxed for 48 hours
  2. customthe precipitate formed
  3. filtrationis filtered off
  4. washwashed with water
  5. customdried under vacuum

出典と根拠

ORDレコード
ord-d68ee45e103d4ea48d0b855e928f69fb
出典データセット
uspto-grants-1999_07
特許番号
US05925768

反応ノート

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