Hydrazine hydrate (1:1) → HCID 4358478、化合物
反応式
[O:1]1[CH2:6][CH2:5][N:4]([C:7](=[O:13])[C:8](OCC)=[O:9])[CH2:3][CH2:2]1.O.[NH2:15][NH2:16]>C(O)C>[O:1]1[CH2:6][CH2:5][N:4]([C:7](=[O:13])[C:8]([NH:15][NH2:16])=[O:9])[CH2:3][CH2:2]1参加物
4
実験手順
Ethyl 2-morpholino-2-oxoacetate (1.0 g, 5.34 mmol) was dissolved in ethanol (7 mL) and hydrazine hydrate (0.267 g, 5.34 mmol) was added dropwise at 0° C. The reaction mixture was stirred at room temperature for 1.5 h. The reaction mixture was concentrated under reduced pressure to give 0.9 g of the crude product, which was used without further purification in the following step. Crude yield 90%. 1H NMR (400 MHz, CDCl3) δ 9.79 (s, 1H), 4.43-4.48 (m, 2H), 3.56-3.61 (m, 4H), 3.40-3.48 (m, 4H). LCMS m/z 174.16 [M+H]+, tR=2.031 min.
後処理
- concentrationThe reaction mixture was concentrated under reduced pressure
出典と根拠
- ORDレコード
- ord-9d7048ae915d4329b31a554b5c2361cb
- 出典データセット
- uspto-grants-2015_08
- 特許番号
- US09096543B2
反応ノート
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