Hydrazine → HCID 20435928、化合物
反応式
[CH3:1][C:2]([CH2:13][CH2:14][O:15][CH:16]1[CH2:21][CH2:20][CH2:19][CH2:18][O:17]1)([C:8](OCC)=[O:9])[C:3](OCC)=[O:4].[NH2:22][NH2:23]>>[CH3:1][C:2]1([CH2:13][CH2:14][O:15][CH:16]2[CH2:21][CH2:20][CH2:19][CH2:18][O:17]2)[C:8](=[O:9])[NH:23][NH:22][C:3]1=[O:4]参加物
3
実験手順
A mixture of 120.8 g (0.4 mol) of diethyl 2-methyl-2-[2-(tetrahydro-2-pyranyloxy)ethyl]-propane-1,3-dioate and 150 ml of anhydrous hydrazine was heated under reflux for 64 hours. The excess hydrazine was removed by distillation and the residue was recrystallized from methanol to give 60.28 g (62%) of 4-methyl-4-[2-(tetrahydro-2-pyranyloxy)-ethyl]-pyrazolidine-3,5-dione having a melting point of 179°-180° C.
後処理
- temperaturewas heated
- temperatureunder reflux for 64 hours
- customThe excess hydrazine was removed by distillation
- customthe residue was recrystallized from methanol
出典と根拠
- ORDレコード
- ord-6d1dba4ee100425ba9a53fd1dda0cf95
- 出典データセット
- uspto-grants-1984_12
- 特許番号
- US04487929
反応ノート
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