Water → 5-Methyl-2-phenylpyrimidine

HRID 1054107

반응식

HRID 1054107 반응식
Cl.[C:2]([NH2:10])(=[NH:9])[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.C(O[CH:14]=[C:15]([CH3:18])[CH:16]=O)C.C[O-].[Na+].O>CO>[CH3:18][C:15]1[CH:14]=[N:9][C:2]([C:3]2[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=2)=[N:10][CH:16]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 80289Benzamidine, hydrochlorideHCID 5591983-Ethoxy-2-methyl-2-propenalHCID 10942334Sodium Methoxide

생성물 1

HCID 8174325-Methyl-2-phenylpyrimidine

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

To a solution of benzamidine hydrochloride (500 mg, 3.19 mmol) and 3-ethoxy-2-methylacrylaldehyde (400 mg, 3.51 mmol) in Methanol (10 mL) was added a NaOMe-solution (30 percent in methanol) dropwise under stirring over 30 minutes. After stirring for 4 hours water (20 mL) was added and mixture was stirred for further 30 minutes at room temperature. After filtration the obtained precipitate was washed with water and dried. White solid. Yield: 220 mg, 41%. 1H NMR (CDCl3, 500 MHz): δH (ppm)=2.34 (s, 3H), 7.44-7.54 (m, 3H), 8.37-8.45 (m, 2H), 8.64 (d, J=0.6 Hz, 2H); 13C NMR (CDCl3, 125 MHz): δC (ppm)=15.7, 128.1, 128.5, 128.8, 130.6, 137.9, 157.6, 162.7; (ESI): m/z=170.97 [M+H]+.

후처리

  1. additionwas added
  2. stirringmixture was stirred for further 30 minutes at room temperature
  3. filtrationAfter filtration the obtained precipitate
  4. washwas washed with water
  5. customdried

출처 및 근거

ORD 기록
ord-b6d8ee63f57f4ca5864e97cf3deebbd2
출처 데이터셋
uspto-grants-2016_07
특허 번호
US09394290B2

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