Hydrazine hydrate (1:1) → (6-Morpholin-4-ylpyrimidin-4-yl)hydrazine

HRID 242247

反応式

HRID 242247 の反応式
Cl[C:2]1[N:7]=[CH:6][N:5]=[C:4]([N:8]2[CH2:13][CH2:12][O:11][CH2:10][CH2:9]2)[CH:3]=1.O.[NH2:15][NH2:16]>C(O)C>[NH:15]([C:2]1[N:7]=[CH:6][N:5]=[C:4]([N:8]2[CH2:13][CH2:12][O:11][CH2:10][CH2:9]2)[CH:3]=1)[NH2:16]

参加物

4

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 7960704-(6-Chloropyrimidin-4-yl)morpholine

生成物 1

HCID 13393622(6-Morpholin-4-ylpyrimidin-4-yl)hydrazine

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

53.0 g (2.7 mmol) 4-(6-chloropyrimidin-4-yl)morpholine are initially introduced into 260 ml ethanol. 132.9 g (2.7 mol) hydrazine hydrate are added and the mixture is stirred under reflux for 16 h. Thereafter, it is cooled to RT and approx. half of the solvent is removed by distillation. The mixture is cooled to 0° C. and the solid formed is filtered off It is rinsed with cold ethanol and the solid is dried first in air and then in vacuo.

後処理

  1. temperatureunder reflux for 16 h
  2. customis removed by distillation
  3. temperatureThe mixture is cooled to 0° C.
  4. customthe solid formed
  5. filtrationis filtered off It
  6. washis rinsed with cold ethanol
  7. customthe solid is dried first in air

出典と根拠

ORDレコード
ord-b52930eea51e4977b80f10005dc45379
出典データセット
uspto-grants-2014_02
特許番号
US08653111B2

関連ノート

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