Phosgene → HCID 19892240、化合物
反応式
[CH3:1][C:2]1([C:5]([NH:7][NH2:8])=[O:6])[CH2:4][CH2:3]1.[C:9](Cl)(Cl)=[O:10]>C(Cl)Cl>[O:10]=[C:9]1[N:8]=[N:7][CH:5]([C:2]2([CH3:1])[CH2:4][CH2:3]2)[O:6]1参加物
4
実験手順
85 gm of 1-methylcyclopropane carboxylic acid hydrazide was added to methylene chloride on a 3-neck 2-liter round bottom flask. The system was first cooled to 0°-5° C. and 590.5 gm of a 12.5% solution of phosgene added dropwise over a period of time. The system was then heated at reflux for 7 hours. The methylene chloride was removed by stripping. The product was washed with petroleum ether and filtered to give 66.6 gm of 2-oxo-5-(1'-methylcyclopropyl)-1,3,4-oxadiazoline as light brown crystals, m.p. 68°-70° C.
後処理
- temperatureThe system was first cooled to 0°-5° C.
- temperatureThe system was then heated
- temperatureat reflux for 7 hours
- customThe methylene chloride was removed by stripping
- washThe product was washed with petroleum ether
- filtrationfiltered
出典と根拠
- ORDレコード
- ord-4be6f102ca8243b8a6947ac6a9da67b2
- 出典データセット
- uspto-grants-1984_01
- 特許番号
- US04426379
反応ノート
読み込み中…