Hydrochloric Acid → (1,4-Diazepan-1-yl)(furan-2-yl)methanone
反応式
[NH:1]1[CH2:7][CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1.Cl.[O:9]1[CH:13]=[CH:12][CH:11]=[C:10]1[C:14](Cl)=[O:15].[OH-].[Na+]>O>[O:9]1[CH:13]=[CH:12][CH:11]=[C:10]1[C:14]([N:1]1[CH2:7][CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1)=[O:15]参加物
6
実験手順
Homopiperazine (70 g) in 160 ml H2O was treated with hydrochloric acid (1 part conc. HCl and 1 part water) until the pH of the solution was 5.5. Furoyl chloride (79.5 g) and 25% NaOH was added simultaneously to maintain a pH between 4.5 and 5.5. Then 50% sodium hydroxide was added until the pH reached 9.5. The solution was extracted with chloroform, dried over potassium carbonate and distilled giving 63.24 g of product. bp 125°-130° C, 10.2mm.
後処理
- temperatureto maintain a pH between 4.5 and 5.5
- extractionThe solution was extracted with chloroform
- dry with materialdried over potassium carbonate
- distillationdistilled
出典と根拠
- ORDレコード
- ord-4929b3f60c5348739be35c8ba7f593ac
- 出典データセット
- uspto-grants-1978_06
- 特許番号
- US04093726
反応ノート
読み込み中…