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

HRID 500882노트

반응식

HRID 500882 반응식
[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

참가 물질

3

반응물 1

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

생성물 1

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

시약·촉매·용매 1

HCID 13387N-methyl-2-pyrrolidone용매

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-06d335ed768f4bf5a193b67e39a0396c
출처 데이터셋
uspto-grants-2010_08
특허 번호
US07772247B2

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