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

HRID 80785ノート

反応式

HRID 80785 の反応式
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

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

反応条件

温度
80 °C

実験手順

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)+

後処理

  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

出典と根拠

ORDレコード
ord-4a7e994b8b1a4fb58a718ba0e2422692
出典データセット
uspto-grants-2014_09
特許番号
US08846656B2

反応ノート

読み込み中…