反応式
C1[CH:6]=[C:5]([S:7][S:8][C:9]2[N:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)N=CC=1.[ClH:15].SCC[NH2:19]>CO>[ClH:15].[N:14]1[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=1[S:8][S:7][CH2:5][CH2:6][NH2:19]参加物
4
実験手順
2,2′-dipyridyldisulfide (13.2 g) was dissolved in 100 ml of methanol. Under vigorously stirring, 3.4 g of 2-mercaptoethylamine hydrochloride in 30 ml of methanol was added dropwise thereto. The reaction mixture was stirred for 1 hour and 40 minutes and the solvent was distilled off. Ethyl acetate was added to the resulting residue for crystallization and crystals were collected by filtration. Crude crystals thus obtained were recrystallized from methanol-ether. The mother liquor was concentrated and crystallized again from ether to obtain 5.62 g of S-(2-pyridylthio)-2-mercaptoethylamine hydrochloride (hereinafter referred to as Compound (2)) (yield 84%). The chemical formula of Compound (2) is shown below.
後処理
- stirringThe reaction mixture was stirred for 1 hour and 40 minutes
- distillationthe solvent was distilled off
- additionEthyl acetate was added to the resulting residue for crystallization and crystals
- filtrationwere collected by filtration
- customCrude crystals thus obtained
- customwere recrystallized from methanol-ether
- concentrationThe mother liquor was concentrated
- customcrystallized again from ether
出典と根拠
- ORDレコード
- ord-6fd4b448e036424e9b5fd4fe736423c6
- 出典データセット
- uspto-grants-2001_09
- 特許番号
- US06291198B1
関連ノート
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