反応式
[O-]CC.[Na+].[Cl:5][C:6]1[CH:14]=[CH:13][C:9]([C:10]([NH2:12])=[NH:11])=[CH:8][CH:7]=1.[C:15](OCC)(=[O:22])[CH2:16][C:17](OCC)=[O:18].Cl>C(O)C>[Cl:5][C:6]1[CH:14]=[CH:13][C:9]([C:10]2[N:12]=[C:17]([OH:18])[CH:16]=[C:15]([OH:22])[N:11]=2)=[CH:8][CH:7]=1参加物
6
反応条件
- 温度
- 40 °C
実験手順
To sodium ethoxide (48 ml of a 21% wt solution in ethanol diluted with a further 130 ml ethanol) was added 4-chlorobenzamidine (8 g) and diethyl malonate (6.67 ml) and the solution left to stir at 40° C. for 96 hrs. The reaction mixture was subsequently cooled to 5° C. and acidified cautiously to pH 2 using concentrated hydrochloric acid. The solid thus precipitated was filtered, washed with excess cold water, then 50 ml diethyl ether and dried in vacuo yielding the title compound (7.51 g).
後処理
- waitthe solution left
- temperatureThe reaction mixture was subsequently cooled to 5° C.
- customThe solid thus precipitated
- filtrationwas filtered
- washwashed with excess cold water
- dry with material50 ml diethyl ether and dried in vacuo
出典と根拠
- ORDレコード
- ord-7724f17f420741168f75f8b88270b3d2
- 出典データセット
- uspto-grants-2005_07
- 特許番号
- US06916804B2
関連ノート
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