3-Heptanone → HCID 252033、化合物

HRID 439610

反応式

HRID 439610 の反応式
[CH3:1][CH2:2][C:3](=O)[CH2:4][CH2:5][CH2:6][CH3:7].Cl.[NH2:10][OH:11]>CO>[CH3:1][CH2:2][C:3](=[N:10][OH:11])[CH2:4][CH2:5][CH2:6][CH3:7]

参加物

4

実験手順

A mixture of 1-azabicyclo 2.2.1!heptan-3-one (8.83 g, 79 mmol) and hydroxylamine hydrochloride (5.52 g, 79 mmol) in MeOH (200 mL) was stirred at 25° C. for 18 hours. The solvent was removed under reduced pressure and the tan solid was partitioned between saturated Na2CO3 and CHCl3. The organic extracts were dried (Na2CO3), and concentrated to give the oxime, 5.48 g, 54.7%. The aqueous layer was concentrated, and re-extracted with CHCl3 to yield another 3.17 g product. Total yield, 8.65 g, 86%. The ratio is from 95% to 98% Z to E.

後処理

  1. additionA mixture of 1-azabicyclo 2.2.1
  2. customThe solvent was removed under reduced pressure
  3. customthe tan solid was partitioned between saturated Na2CO3 and CHCl3
  4. dry with materialThe organic extracts were dried (Na2CO3)
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-c93303fc8c2e49a689a553bfe5c8f4fa
出典データセット
uspto-grants-1996_05
特許番号
US05514812

関連ノート

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