2-Methyl-2-thiopseudourea → Benzyl [amino(methylsulfanyl)methylene]carbamate
反応式
[CH3:1][S:2][C:3](=[NH:5])[NH2:4].[CH2:6]([O:13][C:14](Cl)=[O:15])[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1.[OH-].[Na+]>O>[CH2:6]([O:13][C:14]([NH:5][C:3](=[NH:4])[S:2][CH3:1])=[O:15])[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1参加物
5
実験手順
13.9 g (0.1 mole) of S-methyl-isothiourea are dissolved in 50 ml of water, cooled to a temperature of 0° to 5° C., and at this temperature and with constant stirring 15 ml (0.1 mole) of chloroformic acid benzyl ester and 50 ml of 4 N sodium hydroxide are added in about 20 minutes. The precipitate formed is filtered, washed three times with 50 ml of cold water, then three times with 50 ml of n-hexane, and finally dried over phosphorpentoxide in vacuo. Yield 15.7 g (70 percent) of the named compound. M.p.: 74° to 75° C.; RF1 0.70 to 0.75.
後処理
- temperaturecooled to a temperature of 0° to 5° C.
- additionare added in about 20 minutes
- customThe precipitate formed
- filtrationis filtered
- washwashed three times with 50 ml of cold water
- dry with materialthree times with 50 ml of n-hexane, and finally dried over phosphorpentoxide in vacuo
出典と根拠
- ORDレコード
- ord-a20db19e16264b86af370111a4c273e0
- 出典データセット
- uspto-grants-1982_08
- 特許番号
- US04346078
反応ノート
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