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

HRID 2120556
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HRID 2120556 반응식
[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]
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참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

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온도
95 °C

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-9430fb701f964d5aa151e2579c1689dc
출처 데이터셋
uspto-grants-2004_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06693097B2

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