Thiourea → HCID 178432392、化合物
反応式
C([O:4][CH2:5][C:6]1[CH:11]=[C:10](Cl)[N:9]2[N:13]=[C:14]([CH3:16])[N:15]=[C:8]2[N:7]=1)(=O)C.NC(N)=[S:19]>C(O)C>[OH:4][CH2:5][C:6]1[CH:11]=[C:10]([SH:19])[N:9]2[N:13]=[C:14]([CH3:16])[N:15]=[C:8]2[N:7]=1参加物
4
実験手順
In 600 ml of ethanol was dissolved 31 g of 5-acetoxymethyl-7-chloro-2-methyl-s-triazolo[1,5-a]pyrimidine, and 29.5 g of thiourea was added thereto and the mixture was refluxed for 10 minutes. The reaction mixture was ice-cooled and resulting precipitated crystal was collected by filtration. The crystal was dissolved in 600 ml of a 5 % potassium hydroxide and the mixture was stirred for 30 minutes, ice-cooled and adjusted to pH 2 with 2N hydrochloric acid. Precipitated crystal was collected by filtration, washed with water and dried to obtain 16.33 g of the title compound.
後処理
- additionwas added
- temperaturethe mixture was refluxed for 10 minutes
- temperaturecooled
- customresulting
- customprecipitated crystal
- filtrationwas collected by filtration
- dissolutionThe crystal was dissolved in 600 ml of a 5 % potassium hydroxide
- temperatureice-cooled
- customPrecipitated crystal
- filtrationwas collected by filtration
- washwashed with water
- customdried
出典と根拠
- ORDレコード
- ord-e7f5d73dd3f74d8f91d6c42f429ecb48
- 出典データセット
- uspto-grants-1991_01
- 特許番号
- US04987129
反応ノート
読み込み中…