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Hydrazine → 2-n-Butoxy-4-hydrazino-6-(morpholin-4-yl)pyrimidine

HRID 2262458
ノート
印刷プレビュー

反応式

HRID 2262458 の反応式
[CH2:1]([O:5][C:6]1[N:11]=[C:10](Cl)[CH:9]=[C:8]([N:13]2[CH2:18][CH2:17][O:16][CH2:15][CH2:14]2)[N:7]=1)[CH2:2][CH2:3][CH3:4].[NH2:19][NH2:20]>O1CCOCC1>[CH2:1]([O:5][C:6]1[N:11]=[C:10]([NH:19][NH2:20])[CH:9]=[C:8]([N:13]2[CH2:18][CH2:17][O:16][CH2:15][CH2:14]2)[N:7]=1)[CH2:2][CH2:3][CH3:4]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 9321HydrazineHCID 220469264-(2-Butoxy-6-chloropyrimidin-4-yl)morpholine

生成物 1

HCID 220469222-n-Butoxy-4-hydrazino-6-(morpholin-4-yl)pyrimidine収率 81%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

反応条件

温度
95 °C

実験手順

To a solution of 2-n-butoxy-4-chloro-6-(morpholin-4-yl)pyrimidine (1.38 g, 5.1 mmol) in dioxane (50 ml), anhydrous hydrazine (1.6 mL, 50 mmol) was added. The obtained reaction mixture was heated to 95° C., and stirred for 12 h under N2. After cooling to room temperature, the reaction mixture was quenched with ice-brine and extracted with EtOAc (200 mL). The organic extract was washed with brine, water, and dried over Na2SO4. The solvent was removed under reduced pressure. The crude residue was recrystallized from methanol to obtain 2-n-butoxy-4-hydrazino-6-(morpholin-4-yl)pyrimidine as white crystals (1.10 g, 81%).

後処理

  1. customThe obtained reaction mixture
  2. temperatureAfter cooling to room temperature
  3. customthe reaction mixture was quenched with ice-brine
  4. extractionextracted with EtOAc (200 mL)
  5. extractionThe organic extract
  6. washwas washed with brine, water
  7. dry with materialdried over Na2SO4
  8. customThe solvent was removed under reduced pressure
  9. customThe crude residue was recrystallized from methanol

出典と根拠

ORDレコード
ord-0947510496f04e029c2b6ab9cdef6eb5
出典データセット
uspto-grants-2010_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07851466B2

反応ノート

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