3-Amino-1-propanol → 3-[(2-Chloro-5-methyl-4-pyrimidinyl)amino]-1-propanol

HRID 2235948노트

반응식

HRID 2235948 반응식
[Cl:1][C:2]1[N:7]=[C:6](Cl)[C:5]([CH3:9])=[CH:4][N:3]=1.[NH2:10][CH2:11][CH2:12][CH2:13][OH:14].C(=O)([O-])[O-].[Na+].[Na+]>C(O)C>[Cl:1][C:2]1[N:7]=[C:6]([NH:10][CH2:11][CH2:12][CH2:13][OH:14])[C:5]([CH3:9])=[CH:4][N:3]=1

참가 물질

5

반응물 3

HCID 90863-Amino-1-propanolHCID 10340Sodium CarbonateHCID 74508Pyrimidine, 2,4-dichloro-5-methyl-

생성물 1

HCID 593004463-[(2-Chloro-5-methyl-4-pyrimidinyl)amino]-1-propanol수율 99%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To a solution of 2,4-dichloro-5-methylpyrimidine (8.00 g, 49.1 mmol) and 3-amino-1-propanol (4.50 mL, 58.9 mmol) in ethanol (200 mL) was added sodium carbonate (26.0 g, 245 mmol). The solution was vigorously stirred at rt for 24 h. The mixture was filtered over Celite® and the filtrate concentrated under reduced pressure. The resulting solid was triturated with Et2O to give the product as a white solid (9.80 g, 99%). 1H NMR (400 MHz, CDCl3) δ 1.86 (qt, 2H), 2.00 (s, 3H), 3.55 (t, 2H), 3.64 (t, 2H), 4.92 (broad, 2H), 7.68 (s, 1H).

후처리

  1. filtrationThe mixture was filtered over Celite®
  2. concentrationthe filtrate concentrated under reduced pressure
  3. customThe resulting solid was triturated with Et2O

출처 및 근거

ORD 기록
ord-522ea5aec6e14a68ab564a89daffd90e
출처 데이터셋
uspto-grants-2010_05
특허 번호
US07714004B2

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