Potassium Hydroxide → N-(2-morpholinophenyl)cyanamide

HRID 1492277ノート

反応式

HRID 1492277 の反応式
[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

  1. temperaturethe mixture heated
  2. temperatureunder reflux for 10 minutes
  3. temperaturecooled to ambient temperature
  4. filtrationThe mixture was filtered
  5. customThe solid which formed
  6. customwas separated by filtration
  7. washwashed with water
  8. 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

読み込み中…