Hydrochloric Acid → HCID 178481676、化合物

HRID 1045674ノート

反応式

HRID 1045674 の反応式
C(O[C:4](=[O:20])[CH2:5][C:6](=O)[C:7]1[CH:12]=[CH:11][N:10]=[C:9]([C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)[N:8]=1)C.[CH3:21][NH:22][C:23]([NH2:25])=[S:24].N12CCCN=C1CCCCC2.Cl>C(O)C>[SH:24][C:23]1[N:22]([CH3:21])[C:4](=[O:20])[CH:5]=[C:6]([C:7]2[CH:12]=[CH:11][N:10]=[C:9]([C:13]3[CH:14]=[CH:15][CH:16]=[CH:17][CH:18]=3)[N:8]=2)[N:25]=1

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 811841,8-Diazabicyclo(5.4.0)undec-7-eneHCID 2723704MethylthioureaHCID 578700193-Oxo-3-(2-phenyl-pyrimidin-4-yl)-propionic acid ethyl ester

生成物 1

HCID 178481676HCID 178481676、化合物収率 93%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒2 回

実験手順

A solution of 3-oxo-3-(2-phenyl-pyrimidin-4-yl)-propionic acid ethyl ester (2.74 g, 10.1 mmol), N-methylthiourea (1.39 g, 15.5 mmol) and 1,8-diazabicyclo[5,4,0]undec-7-en (1.57 g, 10.3 mmol) in ethanol (30 ml) was heated under reflux for 18 hours. After the solution was acidified by addition of hydrochloric acid, ethanol was removed under reduced pressure, and the resulting solid was filtered, washed with water and dried to afford 2-mercapto-1-methyl-2′-phenyl-1H-[4,4′]bipyrimidinyl-6-one (2.78 g, 93%).

後処理

  1. temperatureunder reflux for 18 hours
  2. customwas removed under reduced pressure
  3. filtrationthe resulting solid was filtered
  4. washwashed with water
  5. customdried

出典と根拠

ORDレコード
ord-f8f3e04793db47c2ad9eac4b63976e5b
出典データセット
uspto-grants-2013_10
特許番号
US08569294B2

反応ノート

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