Water → HCID 23348537、化合物
反応式
[OH-].[Na+].O.[S:4]1[CH:8]=[CH:7][CH:6]=[C:5]1[C:9]1([CH2:14][NH2:15])[CH2:13][CH2:12][CH2:11][CH2:10]1.ClC(OCC)=O.[C:22](=S)=[S:23]>>[S:4]1[CH:8]=[CH:7][CH:6]=[C:5]1[C:9]1([CH2:14][N:15]=[C:22]=[S:23])[CH2:13][CH2:12][CH2:11][CH2:10]1参加物
実験手順
A solution of 21.2 parts of sodium hydroxide in 500 parts of water is cooled to 10° C. and there is added successively 45.6 parts of carbon disulfide and then dropwise 95.83 parts of 1-(2-thienyl)-cyclopentanemethylamine (exothermic reaction). After the addition is complete, the whole is stirred for 30 minutes at room temperature. Then there are added 57.5 parts of ethyl chloroformate at 30° C. (exothermic reaction: cooling is necessary). The whole is stirred for 3 hours at 50° C. and further stirred overnight without heating. The product is extracted with benzene. The extract is dried, filtered and evaporated. The residue is poured onto 350 parts of water and the whole is heated for 3 hours at 80°-90° C. The mixture is cooled and the product is extracted with dichloromethane. The extract is dried, filtered and evaporated. The oily residue is distilled twice, yielding 88 parts of [1-(2-thienyl)cyclopentylmethyl]isothiocyanate; bp. 110° C. at 0.1 mm pressure; nD20 :1.5960; d2020 :1.1743.
後処理
- additionAfter the addition
- custom(exothermic reaction: cooling is necessary)
- stirringThe whole is stirred for 3 hours at 50° C. and further stirred overnight
- temperaturewithout heating
- extractionThe product is extracted with benzene
- customThe extract is dried
- filtrationfiltered
- customevaporated
- additionThe residue is poured onto 350 parts of water
- temperaturethe whole is heated for 3 hours at 80°-90° C
- temperatureThe mixture is cooled
- extractionthe product is extracted with dichloromethane
- customThe extract is dried
- filtrationfiltered
- customevaporated
- distillationThe oily residue is distilled twice
出典と根拠
- ORDレコード
- ord-29421ad13992487a9747e93a86cf5509
- 出典データセット
- uspto-grants-1980_08
- 特許番号
- US04216217
反応ノート
読み込み中…