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Acetic Acid → 2-(N-(2-bromo-4-(2-propyl)phenyl)-N-ethylamino)-4-(morpholinomethyl)-6-methylpyrimidine

HRID 1251480
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HRID 1251480 반응식
[Br:1][C:2]1[CH:7]=[C:6]([CH:8]([CH3:10])[CH3:9])[CH:5]=[CH:4][C:3]=1[N:11]([CH2:27][CH3:28])[C:12]1[N:17]=[C:16]([CH3:18])[CH:15]=[C:14]([C:19]([N:21]2[CH2:26][CH2:25][O:24][CH2:23][CH2:22]2)=O)[N:13]=1.B.C(O)(=O)C.[OH-].[Na+]>C1COCC1.CCOC(C)=O>[Br:1][C:2]1[CH:7]=[C:6]([CH:8]([CH3:10])[CH3:9])[CH:5]=[CH:4][C:3]=1[N:11]([CH2:27][CH3:28])[C:12]1[N:13]=[C:14]([CH2:19][N:21]2[CH2:22][CH2:23][O:24][CH2:25][CH2:26]2)[CH:15]=[C:16]([CH3:18])[N:17]=1
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참가 물질

7

반응물 4

HCID 176Acetic AcidHCID 6331BoraneHCID 14798Sodium HydroxideHCID 15490843N-(2-Bromo-4-(1-Methylethyl)Phenyl)-N-Ethyl-4-Methyl-6-(4-Morpholinylcarbonyl)-2-Pyrimidinamine

생성물 1

HCID 102522822-(N-(2-bromo-4-(2-propyl)phenyl)-N-ethylamino)-4-(morpholinomethyl)-6-methylpyrimidine수율 40.2%

시약·촉매·용매 2

HCID 8028
Tetrahydrofuran
용매
2회
HCID 8857Ethyl Acetate용매

실험 절차

A solution of N-(2-bromo-4-(1-methylethyl)phenyl)-N-ethyl-4-methyl-6-(4-morpholinylcarbonyl)-2-pyrimidinamine (750 mg, 1.72 mmol) in anhydrous THF (1.4 mL) was stirred at ambient temperature under a nitrogen atmosphere. A solution of borane in THF (1 M, 3.6 mL, 3.6 mmol) was added dropaise. The reaction mixture was then warmed to reflux temperature and stirred for 20 hours. After cooling to room temperature, acetic acid (3.5 mL) was added slowly and the mixture was heated to reflux temperature and stirred for 30 min. After being cooled to ambient temperature, the reaction mixture was poured onto a 3N NaOH solution, mixed and extracted three times with EtOAc. The combined organic layers were dried over MgSO4, filtered and concentrated in vacuo. Column chromatography (EtOAc) of the residue afforded the title compound as an oil (300 mg, 39% yield, Rf 0.3): NMR (CDCl3, 300 MHz): d 7.5 (s, 1H), 7.2 (d, 1H, J=7), 7.15 (d, 1H, J=7), 6.5 ( s, 1H), 4.3-4.1 (m, 1H), 3.8-3.6 (m, 7H), 3.5-3.3 (m, 2H),2.9 (septet, 1H, J=7), 2.55-2.35 (br m, 3H), 2.35-2.25 ( m, 2H), 1.3 (d, 6H, J=7), 1.2 (t, 3H, J=7); CI-HRMS: calcd: 433.1603 (M+H), found: 433.1586.

후처리

  1. temperatureThe reaction mixture was then warmed
  2. temperatureto reflux temperature
  3. temperaturethe mixture was heated
  4. temperatureto reflux temperature
  5. stirringstirred for 30 min
  6. temperatureAfter being cooled to ambient temperature
  7. additionmixed
  8. extractionextracted three times with EtOAc
  9. dry with materialThe combined organic layers were dried over MgSO4
  10. filtrationfiltered
  11. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-e1874f0b7d2d491f9f7d987c431ffc7d
출처 데이터셋
uspto-grants-2002_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06342503B1

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