4-Chloro-6-(phenylethynyl)pyrimidin-5-amine → 4-Chloro-6-phenyl-5H-pyrrolo[3,2-d]pyrimidine

HRID 500882ノート

反応式

HRID 500882 の反応式
[Cl:1][C:2]1[C:7]([NH2:8])=[C:6]([C:9]#[C:10][C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)[N:5]=[CH:4][N:3]=1>CN1C(=O)CCC1>[Cl:1][C:2]1[C:7]2[NH:8][C:10]([C:11]3[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=3)=[CH:9][C:6]=2[N:5]=[CH:4][N:3]=1

参加物

3

反応物 1

HCID 594245784-Chloro-6-(phenylethynyl)pyrimidin-5-amine

生成物 1

HCID 573550364-Chloro-6-phenyl-5H-pyrrolo[3,2-d]pyrimidine

試薬・触媒・溶媒 1

HCID 13387N-methyl-2-pyrrolidone溶媒

実験手順

To a solution of 251 (30.8 mg, 0.134 mmol) in NMP (1.4 mL) a suspension of KH in mineral oil (35%, 31 mL, 0.268 mmol) was added in one portion. The mixture was stirred at room temperature overnight and partitioned between EtOAc and water. The organic phase was collected, dried over anhydrous Na2SO4 and concentrated. The residue was purified by flash chromatography, eluent EtOAc/hexane (1:2) to afford title compound affording 252 (22.7 mg, 74% yield). MS (m/z): 230.1 (100%) 232.1 (33%) (M+1).

後処理

  1. additionwas added in one portion
  2. custompartitioned between EtOAc and water
  3. customThe organic phase was collected
  4. dry with materialdried over anhydrous Na2SO4
  5. concentrationconcentrated
  6. customThe residue was purified by flash chromatography, eluent EtOAc/hexane (1:2)

出典と根拠

ORDレコード
ord-06d335ed768f4bf5a193b67e39a0396c
出典データセット
uspto-grants-2010_08
特許番号
US07772247B2

反応ノート

読み込み中…