Cysteamine Hydrochloride → HCID 22253943、化合物
反応式
Cl.[NH2:2][CH2:3][CH2:4][SH:5].[C:6]([Cl:12])(=[O:11])[C:7]([CH3:10])([CH3:9])[CH3:8]>>[ClH:12].[CH3:8][C:7]([CH3:10])([CH3:9])[C:6](=[O:11])[S:5][CH2:4][CH2:3][NH2:2]参加物
3
実験手順
A solution of cysteamine hydrochloride (30.81 mmol) in pivaloyl chloride (10 mL) was heated to 100° C. during 15 minutes. The reaction mixture was allowed to cool down to room temperature and was triturated in Et2O. The mixture was filtered. The solid was washed with Et2O and then dissolved in DMF (50 mL and 5 drops of HCl) upon heating. After cooled down to room temperature, the mixture was precipitated with Et2O, filtered and washed with Et2O to give after drying under vacuum the expected compound as a white solid in 94% yield. 1H NMR (DMSO-d6, 400 MHz) δ (ppm) 1.19 (s, 9H), 2.88 (t, J=7.08 Hz, 2H), 3.05-3.08 (m, 2H), 8.30 (s, 3H).
後処理
- customwas triturated in Et2O
- filtrationThe mixture was filtered
- washThe solid was washed with Et2O
- dissolutiondissolved in DMF (50 mL and 5 drops of HCl)
- temperatureupon heating
- temperatureAfter cooled down to room temperature
- customthe mixture was precipitated with Et2O
- filtrationfiltered
- washwashed with Et2O
- customto give
- dry with materialafter drying under vacuum the expected compound as a white solid in 94% yield
出典と根拠
- ORDレコード
- ord-4dadf182d78d4490bd7b5fb27108eeac
- 出典データセット
- uspto-grants-2015_08
- 特許番号
- US09109001B2
反応ノート
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