4-Amino-2-methyl-5-pyrimidinemethanamine → HCID 54724214, 화합물

HRID 1831992

반응식

HRID 1831992 반응식
[OH:1][C:2]1[CH:7]=[C:6]([CH3:8])O[C:4](=[O:9])[CH:3]=1.[NH2:10][C:11]1[C:16]([CH2:17][NH2:18])=[CH:15][N:14]=[C:13]([CH3:19])[N:12]=1>O>[NH2:10][C:11]1[C:16]([CH2:17][N:18]2[C:6]([CH3:8])=[CH:7][C:2]([OH:1])=[CH:3][C:4]2=[O:9])=[CH:15][N:14]=[C:13]([CH3:19])[N:12]=1

참가 물질

4

반응물 2

HCID 667624-Amino-2-methyl-5-pyrimidinemethanamineHCID 546757574-Hydroxy-6-methyl-2-pyrone

생성물 1

HCID 54724214HCID 54724214, 화합물수율 58.6%

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
100 °C

실험 절차

A mixture of 4-hydroxy-6-methyl-2-pyrone (0.9 g, 0.007 mol) and 4-amino-5-aminomethyl-2-methylpyrimidine (1.0 g, 0.007 mol) in water (10.0 ml) was heated at 100° C. for 1 h under argon atmosphere. The reaction mixture was cooled, and filtered the yellow precipitate. It was washed successively with cold water, ethanol, and dried in vacuo to afford the title compound (1.01 g, 51%) as a pale yellow powder: 1H NMR (DMSO-d6/400 MHz) δ 7.62 (s, 1H), 7.04 (s, 1H), 5.83 (d, 1H, J=2.0 Hz), 5.58 (d, 1H, J=2.0 Hz), 4.92 (s, 2H), 2.24 (s, 3H), and 2.22 (s, 3H); ES-HRMS m/z 325.0304 (M+H C12H14N4O2Br requires 325.0295). Step 2 1-[(4-amino-2-methylpyrimidin-5-yl)methyl]-3-bromo-4-hydroxy-6-methylpyridin-2(1H)-one

후처리

  1. temperatureThe reaction mixture was cooled
  2. filtrationfiltered the yellow precipitate
  3. washIt was washed successively with cold water, ethanol
  4. customdried in vacuo

출처 및 근거

ORD 기록
ord-3dba739c2a4d4cffbeddd87551f97052
출처 데이터셋
uspto-grants-2006_06
특허 번호
US07067540B2

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