Water → (6-Chloro-5-methylpyridin-3-yl)methanamine hydrochloride
反応式
[N:1]([CH2:4][C:5]1[CH:6]=[C:7]([CH3:12])[C:8]([Cl:11])=[N:9][CH:10]=1)=[N+]=[N-].C1C=CC(P(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1.O>C1COCC1>[ClH:11].[Cl:11][C:8]1[N:9]=[CH:10][C:5]([CH2:4][NH2:1])=[CH:6][C:7]=1[CH3:12]参加物
5
実験手順
To the solution of 5-(azidomethyl)-2-chloro-3-methylpyridine 30-3 (2.0 g, 11 mmol) in THF (20 mL) was added PPh3 (3.17, 12 mmol) slowly. After 2 hours, H2O was added to the reaction mixture and the reaction was stirred for additional 15 hours, and the solvent was removed. The crude product was partitioned between ethyl acetate (50 mL) and 0.2 N HCl (50 mL). The aqueous phase was dried to give (6-chloro-5-methylpyridin-3-yl)methanamine HCl salt 30-4 as a white solid.
後処理
- customthe solvent was removed
- customThe crude product was partitioned between ethyl acetate (50 mL) and 0.2 N HCl (50 mL)
- customThe aqueous phase was dried
出典と根拠
- ORDレコード
- ord-ef5dfc70a84f455cb88af2762191b626
- 出典データセット
- uspto-grants-2015_11
- 特許番号
- US09181235B2
反応ノート
読み込み中…