反応式
[C:1]([CH2:3][C:4]([OH:6])=O)#[N:2].[NH2:7][C:8]1[S:9][CH:10]=[CH:11][N:12]=1.C1(N=C=NC2CCCCC2)CCCCC1>C(#N)C.[OH-].[Na+]>[C:1]([CH2:3][C:4]([NH:7][C:8]1[S:9][CH:10]=[CH:11][N:12]=1)=[O:6])#[N:2]参加物
6
実験手順
4.5 g of cyanoacetic acid and 5.3 g of 2-aminothiazole, each in acetonitrile were combined, and the suspension (60 ml) was treated with a solution of 12.0 g of dicyclohexylcarbodiimide in 30 ml of acetonitrile. After exothermic reaction (and solidification) additional acetonitrile (60 ml) was added and the mixture stirred 1 hr and let stand overnight. The collected solid (20 g) was stirred with dilute (ca. 2%) NaOH solution and filtered. The filtrate was acidified with 6 N HCl and the product collected, washed with water, dried (m.p. 229°-230°) and recrystallized from acetone to give 2-(cyanoacetylamino)thiazole, m.p. 231°-2° dec.
後処理
- additionwas added
- waitlet stand overnight
- filtrationfiltered
- customthe product collected
- washwashed with water
- customdried (m.p. 229°-230°)
- customrecrystallized from acetone
出典と根拠
- ORDレコード
- ord-7aed9a92fe354bd6b93832256714feb2
- 出典データセット
- uspto-grants-1984_03
- 特許番号
- US04435407
関連ノート
読み込み中…