反応式
Cl.[NH2:2][CH2:3][CH2:4][SH:5].N.[CH2:7](Br)[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1>CO>[CH2:7]([S:5][CH2:4][CH2:3][NH2:2])[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1参加物
5
実験手順
To a suspension of 0.1 mole cysteamine hydrochloride in 20 mL methanol were added 13.6 mL of 25% ammonia solution, followed by dropwise addition of 0.12 mole benzyl bromide at room temperature. The mixture was stirred for 0.5 h, and the formed precipitate of S-dibenzylcysteamine was collected by filtration. The product was extracted with ether (3×100 mL) and the organic phase was successively washed with brine (2×100 mL), dried over MgSO4 and the solvent evaporated in vacuo. The crude product was essentially pure enough for the next step. It could, however be recrystallized from ethyl acetate. Yield 86%, of white solid. m.p. 85–6° C. NMR (CDCl3) in agreement with the title compound.
後処理
- filtrationthe formed precipitate of S-dibenzylcysteamine was collected by filtration
- extractionThe product was extracted with ether (3×100 mL)
- washthe organic phase was successively washed with brine (2×100 mL)
- dry with materialdried over MgSO4
- customthe solvent evaporated in vacuo
- customIt could, however be recrystallized from ethyl acetate
出典と根拠
- ORDレコード
- ord-40c021b30b0b44aeab08b6c10bded196
- 出典データセット
- uspto-grants-2006_08
- 特許番号
- US07084244B2
関連ノート
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