Hydrochloric Acid → 1-methyl-2-((2R)-2-methyl-piperazin-1-yl)-1H-[4,4']bipyrimidinyl-6-one

HRID 1045692ノート

反応式

HRID 1045692 の反応式
C(OC([N:8]1[CH2:13][CH2:12][N:11]([C:14]2[N:15]([CH3:27])[C:16](=[O:26])[CH:17]=[C:18]([C:20]3[CH:25]=[CH:24][N:23]=[CH:22][N:21]=3)[N:19]=2)[C@H:10]([CH3:28])[CH2:9]1)=O)(C)(C)C.Cl>C(OCC)(=O)C>[CH3:27][N:15]1[C:16](=[O:26])[CH:17]=[C:18]([C:20]2[CH:25]=[CH:24][N:23]=[CH:22][N:21]=2)[N:19]=[C:14]1[N:11]1[CH2:12][CH2:13][NH:8][CH2:9][C@H:10]1[CH3:28]

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 57870141(3R)-3-methyl-4-(1-methyl-6-oxo-1,6-dihydro-[4,4']bipyrimidinyl-2-yl)-piperazine-1-carboxylic acid tert-butyl ester

生成物 1

HCID 250045961-methyl-2-((2R)-2-methyl-piperazin-1-yl)-1H-[4,4']bipyrimidinyl-6-one収率 91%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒2 回

実験手順

To a solution of (3R)-3-methyl-4-(1-methyl-6-oxo-1,6-dihydro-[4,4′]bipyrimidinyl-2-yl)-piperazine-1-carboxylic acid tert-butyl ester (6.9 g, 18 mmol) in ethyl acetate (35 ml) was added hydrogen chloride (4N) in ethyl acetate (35 ml) at room temperature. The mixture was stirred at room temperature for 2 hours and was concentrated under reduced pressure. The residue was partitioned between aqueous sodium hydrogen carbonate and chloroform, and the organic layer was dried over sodium sulfate. The solvent was evaporated under reduced pressure to afford 1-methyl-2-((2R)-2-methyl-piperazin-1-yl)-1H-[4,4′]bipyrimidinyl-6-one (4.6 g, 91%).

後処理

  1. concentrationwas concentrated under reduced pressure
  2. customThe residue was partitioned between aqueous sodium hydrogen carbonate and chloroform
  3. dry with materialthe organic layer was dried over sodium sulfate
  4. customThe solvent was evaporated under reduced pressure

出典と根拠

ORDレコード
ord-eb473c79e5984026af4910fb632d4ed7
出典データセット
uspto-grants-2013_10
特許番号
US08569294B2

反応ノート

読み込み中…