Methyl 4-methyl-3-oxopentanoate → 1-(2-(2,6-dimethylphenyl)-4-methoxy-7,8-dihydropyrido[4,3-d]pyrimidin-6(5H)-yl)-4-methylpentane-1,3-dione

HRID 80765

반응식

HRID 80765 반응식
[CH3:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([CH3:8])[C:3]=1[C:9]1[N:10]=[C:11]([O:19][CH3:20])[C:12]2[CH2:18][NH:17][CH2:16][CH2:15][C:13]=2[N:14]=1.[CH3:21][CH:22]([CH3:30])[C:23](=[O:29])[CH2:24][C:25](OC)=[O:26]>CN(C1C=CN=CC=1)C.C1(C)C=CC=CC=1>[CH3:8][C:4]1[CH:5]=[CH:6][CH:7]=[C:2]([CH3:1])[C:3]=1[C:9]1[N:10]=[C:11]([O:19][CH3:20])[C:12]2[CH2:18][N:17]([C:25](=[O:26])[CH2:24][C:23](=[O:29])[CH:22]([CH3:30])[CH3:21])[CH2:16][CH2:15][C:13]=2[N:14]=1

참가 물질

5

반응물 2

HCID 2759969Methyl 4-methyl-3-oxopentanoateHCID 712446992-(2,6-Dimethylphenyl)-4-methoxy-5,6,7,8-tetrahydropyrido[4,3-d]pyrimidine

생성물 1

HCID 866902521-(2-(2,6-dimethylphenyl)-4-methoxy-7,8-dihydropyrido[4,3-d]pyrimidin-6(5H)-yl)-4-methylpentane-1,3-dione

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매HCID 1140Toluene용매

반응 조건

온도
150 °C

실험 절차

A mixture of 2-(2,6-dimethylphenyl)-4-methoxy-5,6,7,8-tetrahydropyrido[4,3-d]pyrimidine (4.8 g, 17.82 mmol), methyl 4-methyl-3-oxopentanoate (5.14 g, 35.6 mmol), and DMAP (0.327 g, 2.67 mmol) was dissolved in toluene (70 mL). The mixture was evenly divided into four 20 mL microwave vials. Each vial was heated to 150° C. for 30 min via microwave irradiation. The reaction mixtures were combine and directly concentrated. The resulting residue was purified via silica gel FCC (0-80% EtOAc/heptane) to give 1-(2-(2,6-dimethylphenyl)-4-methoxy-7,8-dihydropyrido[4,3-d]pyrimidin-6(5H)-yl)-4-methylpentane-1,3-dione. MS (ESI+) m/z 382.3 (M+H)+.

후처리

  1. customThe reaction mixtures
  2. concentrationdirectly concentrated
  3. customThe resulting residue was purified via silica gel FCC (0-80% EtOAc/heptane)

출처 및 근거

ORD 기록
ord-2d40f3e3235141af880e9afa258ab03e
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08846656B2

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