Hydrogen Sulfide → HCID 19848484、化合物
反応式
N1CCCCC1.[OH-].C([N+](C)(C)C)C1C=CC=CC=1.[CH:19]([N:21]([CH2:25][CH:26]=[CH2:27])[CH2:22][CH:23]=[CH2:24])=[O:20].[SH2:28]>CO>[CH:19]([N:21]1[CH2:25][CH:26]([CH3:27])[S:28][CH:23]([CH3:24])[CH2:22]1)=[O:20]参加物
6
実験手順
Piperidine (10 ml) and 10 ml of a 40% solution of benzyltrimethylammoniumhydroxide in methanol were added to a solution of N-formyl-diallylamine (55 g) in methanol (200 ml). Hydrogen sulfide (50 g) was introduced into the resulting solution, and unreacted hydrogen sulfide was kept at reflux for 7 hours by means of "cold finger". The mixture was left at room temperature for 48 hours, flushed with nitrogen, diluted with ether, and washed with water. The organic phase was dried, and the solvent evaporated in vacuo. Distillation of the residue gave the title compound with boiling point 145° C./15 mmHg.
後処理
- temperatureat reflux for 7 hours by means of "cold finger"
- customflushed with nitrogen
- additiondiluted with ether
- washwashed with water
- customThe organic phase was dried
- customthe solvent evaporated in vacuo
- distillationDistillation of the residue
出典と根拠
- ORDレコード
- ord-e0c489c0daac4c04bbda3865cc1b37aa
- 出典データセット
- uspto-grants-1989_09
- 特許番号
- US04870063
反応ノート
読み込み中…