Isopropanol → 5H,6H,7H,8H-pyrido(4,3-d)pyrimidine

HRID 80785노트

반응식

HRID 80785 반응식
C([N:8]1[CH2:19][CH2:18][C:11]2[N:12]=[C:13](Cl)[N:14]=[C:15](Cl)[C:10]=2[CH2:9]1)C1C=CC=CC=1.Cl.Cl.C[C@H]1CN[C@H](C)CN1.CCN(C(C)C)C(C)C.CC(O)C>C(OCC)C>[N:12]1[C:11]2[CH2:18][CH2:19][NH:8][CH2:9][C:10]=2[CH:15]=[N:14][CH:13]=1

참가 물질

6

반응물 4

HCID 3776IsopropanolHCID 81531DiisopropylethylamineHCID 12285161(trans)-2,5-Dimethylpiperazine dihydrochlorideHCID 378190156-Benzyl-2,4-dichloro-5,6,7,8-tetrahydropyrido(4,3-d)pyrimidine

생성물 1

HCID 109326745H,6H,7H,8H-pyrido(4,3-d)pyrimidine

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

반응 조건

온도
80 °C

실험 절차

A mixture of 6-benzyl-2,4-dichloro-5,6,7,8-tetrahydropyrido[4,3-d]pyrimidine (2.0 g, 6.80 mmol), (trans)-2,5-dimethylpiperazine dihydrochloride (7.63 g, 40.8 mmol), DIEA (15.4 mL, 88 mmol) and iPrOH (180 mL) was heated at 80° C. for 3.5 days. At that time the reaction was diluted with diethyl ether and the solid was removed by filtration. The filtrate was then washed with brine and the organic layer was dried (Na2SO4), filtered and concentrated to provide crude racemic 6-benzyl-2-chloro-4-(trans)-2,5-dimethylpiperazin-1-yl)-5,6,7,8-tetrahydropyrido[4,3-d]pyrimidine, which was then carried to the next step without further purification. MS (ESI+) m/z 372.2 (M+H)+

후처리

  1. customthe solid was removed by filtration
  2. washThe filtrate was then washed with brine
  3. dry with materialthe organic layer was dried (Na2SO4)
  4. filtrationfiltered
  5. concentrationconcentrated

출처 및 근거

ORD 기록
ord-4a7e994b8b1a4fb58a718ba0e2422692
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08846656B2

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