反応式
[CH2:1]([O:8][NH:9][CH:10]1[CH2:15][NH:14][C@H:13]([C:16]#[N:17])[CH2:12][CH2:11]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[C:18]([OH:23])(=[O:22])[C:19]([OH:21])=[O:20]>C(OC(=O)C)C.CC(C)=O>[C:18]([OH:23])(=[O:22])[C:19]([OH:21])=[O:20].[CH2:1]([O:8][NH:9][CH:10]1[CH2:15][NH:14][C@H:13]([C:16]#[N:17])[CH2:12][CH2:11]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1参加物
5
実験手順
The compound of Formula (IX) was reacted with sulphuric acid and sodium triacetoxy borohydride, in presence of suitable solvent such as ethyl acetate and at temperature below −5° C., to provide (2S)-5-[(benzyloxy)amino]-2-cyanopiperidine (X). The compound of Formula (X) was purified by forming oxalate salt. The compound of Formula (X) was reacted with oxalic acid in a mixture of ethylacetate and acetone to provide (2S)-5-[(benzyloxy)amino]-2-cyanopiperidine ethanedioate (1:1) (XI), which was further treated with sodium hydrogen carbonate to obtain purified (2S)-5-[(benzyloxy)amino]-2-cyanopiperidine (XII). The racemic compound (XI) was treated with methanol to obtain pure (2S,5R)-5-[(benzyloxy)amino]-2-cyanopiperidine ethanedioate.
出典と根拠
- ORDレコード
- ord-74a80cbeac854130a1df403569ddc284
- 出典データセット
- uspto-grants-2015_08
- 特許番号
- US09115131B2
関連ノート
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