Water → (S)-2,2,5,5-tetramethyl-1,3-dioxolane-4-carbaldehyde oxime
反応式
[CH3:1][C:2]1([CH3:11])[O:6][C@@H:5]([CH:7]=O)[C:4]([CH3:10])([CH3:9])[O:3]1.[OH2:12].Cl.[NH2:14]O.C([O-])([O-])=O.[Na+].[Na+]>CO>[CH3:1][C:2]1([CH3:11])[O:6][C@@H:5]([CH:7]=[N:14][OH:12])[C:4]([CH3:10])([CH3:9])[O:3]1参加物
6
実験手順
(R)-2,2,5,5-Tetramethyl-1,3-dioxolane-4-carbaldehyde (16 g, 101 mmol) [Burger, A. Synthesis 1989, (2) 93-97] was dissolved in 1:1 methanol:water (250 mL) and hydroxylamine hydrochloride (7.0 g, 101 mmol), and Na2CO3 (5.4 g, 51 mmol) was added. The reaction was stirred at ambient temperature for 2 hours. The methanol was partially removed in vacuo and the aqueous layer was extracted with CH2Cl2, dried, filtered and concentrated to afford (S)-2,2,5,5-tetramethyl-1,3-dioxolane-4-carbaldehyde oxime (13 g, 75 mmol, 74% yield) as an amber oil.
後処理
- customThe methanol was partially removed in vacuo
- extractionthe aqueous layer was extracted with CH2Cl2
- customdried
- filtrationfiltered
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-b226de073f51492e8cc6f65ac7c49221
- 出典データセット
- uspto-grants-2012_07
- 特許番号
- US08212045B2
反応ノート
読み込み中…