Ammonia → HCID 18668788、化合物
反応式
[CH2:1]1[CH2:13][O:12][C:3]2([CH2:8][CH2:7][N:6]([CH2:9][C:10]#[N:11])[CH2:5][CH2:4]2)[O:2]1.N>[Ni]>[NH2:11][CH2:10][CH2:9][N:6]1[CH2:5][CH2:4][C:3]2([O:12][CH2:13][CH2:1][O:2]2)[CH2:8][CH2:7]1参加物
4
実験手順
A suspension of 12.7 g of 4,4-ethylenedioxy-1-piperidineacetonitrile, 1.3 ml of Raney nickel and 113 ml of 2% methanolic solution of ammonia was catalytically hydrogenated at room temperature under 50 atm for 20 hours. After the reaction, the catalyst was filtered off, and the filtrate was concentrated. The resulting pale green liquid was purified by alumina column chromatography [eluting solvent: ethyl acetate→ethyl acetate—methanol (10:1)] to give 10.1 g of a colorless liquid.
後処理
- customAfter the reaction
- filtrationthe catalyst was filtered off
- concentrationthe filtrate was concentrated
- customThe resulting pale green liquid was purified by alumina column chromatography [eluting solvent: ethyl acetate→ethyl acetate—methanol (10:1)]
出典と根拠
- ORDレコード
- ord-80eab6727b4b4bb39dad5bc0f5280330
- 出典データセット
- uspto-grants-2003_02
- 特許番号
- US06518265B1
反応ノート
読み込み中…