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
70 g. hexahydro-1,4-diazepine was dissolved in 160 ml. water. Hydrochloric acid (20%) was added until the pH was 5.5. Using a pH meter to keep the pH between 4.5 and 5.5, 79.5 g. furoyl chloride was added in portions along with 25% sodium hydroxide. After addition, 50% sodium hydroxide was added to raise the pH to 9.5. The solution was extracted with chloroform 4 times, the chloroform extracts dried over anhydrous potassium carbonates and the solution distilled giving 53.24 g. product. b.p. 125° - 130°
後処理
- additionwas added
- temperatureto raise the pH to 9.5
- extractionThe solution was extracted with chloroform 4 times
- dry with materialthe chloroform extracts dried over anhydrous potassium carbonates
- distillationthe solution distilled
- customgiving 53.24 g
出典と根拠
- ORDレコード
- ord-0fc6127f064641638645cc30feb5fa5d
- 出典データセット
- uspto-grants-1977_08
- 特許番号
- US04044135
反応ノート
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