Potassium Hydroxide → N-(2-morpholinophenyl)cyanamide
反応式
[O:1]1[CH2:6][CH2:5][N:4]([C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][C:8]=2[NH:13][C:14]([NH2:16])=S)[CH2:3][CH2:2]1.[OH-].[K+].O.O.O.C([O-])(=O)C.[Pb+2].C([O-])(=O)C>O>[O:1]1[CH2:2][CH2:3][N:4]([C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][C:8]=2[NH:13][C:14]#[N:16])[CH2:5][CH2:6]1参加物
5
反応条件
- 温度
- 90 °C
実験手順
1-(2-morpholinophenyl)thiourea (10.6 g) was suspended in boiling water (80 ml) and a solution of potassium hydroxide (25.2 g) in hot water (70 ml) was added. The mixture was heated to 90° C. and aliquot portions of a hot solution of lead acetate trihydrate (17.5 g) in water (80 ml) added and the mixture heated under reflux for 10 minutes and cooled to ambient temperature. The mixture was filtered and the filtrate acidified with acetic acid to pH 6. The solid which formed was separated by filtration, washed with water and recrystallised from ethylacetate to give N-(2-morpholinophenyl)cyanamide (m.p. 175°-176° C.).
後処理
- temperaturethe mixture heated
- temperatureunder reflux for 10 minutes
- temperaturecooled to ambient temperature
- filtrationThe mixture was filtered
- customThe solid which formed
- customwas separated by filtration
- washwashed with water
- customrecrystallised from ethylacetate
出典と根拠
- ORDレコード
- ord-d957ba0cc2704dbcaa2affdfdf0bde80
- 出典データセット
- uspto-grants-1994_12
- 特許番号
- US05373008
反応ノート
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