Cyanamide → HCID 178512247、化合物
反応式
[CH:1]1([N:7]=[C:8]=[N:9][C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[N:16]#[C:17][NH2:18]>ClCCCl>[C:17]([NH:18][C:8]([NH:7][CH:1]1[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6]1)=[N:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1)#[N:16]参加物
4
実験手順
A solution of 1.8 g N-cyclohexyl-N'-phenylcarbodiimide [prepared in accordance with Tetrahedron Letters 26, 1661 (1985) in 20 ml of 1,2-dichloroethane is reacted with 0.42 g of cyanamide and the reaction mixture is worked up as described in Example 1. The viscous oily crude product is chromatographed on silica gel (elution with a 4:1 mixture of methylene chloride/diethyl ether), affording a crystalline product which melts at 147°-147.5° C. (recrystallisation from ethyl acetate).
後処理
- customThe viscous oily crude product is chromatographed on silica gel (
- washelution
- additionwith a 4:1 mixture of methylene chloride/diethyl ether),
- customaffording
- customa crystalline product which melts at 147°-147.5° C. (recrystallisation from ethyl acetate)
出典と根拠
- ORDレコード
- ord-2b65effad5414b19839b3a53cc88543f
- 出典データセット
- uspto-grants-1989_08
- 特許番号
- US04859761
反応ノート
読み込み中…