Hydrazine hydrate (1:1) → HCID 178503430, 화합물

HRID 1809680노트

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HRID 1809680 반응식
[Cl:1][C:2]1[N:7]=[C:6](Cl)[C:5]([C:9]([C:11]2[CH:16]=[CH:15][N:14]=[C:13]([S:17][CH3:18])[N:12]=2)=O)=[CH:4][N:3]=1.O.[NH2:20][NH2:21].CCN(C(C)C)C(C)C>C1COCC1>[Cl:1][C:2]1[N:7]=[C:6]2[NH:20][N:21]=[C:9]([C:11]3[CH:16]=[CH:15][N:14]=[C:13]([S:17][CH3:18])[N:12]=3)[C:5]2=[CH:4][N:3]=1

참가 물질

5

반응물 3

HCID 24654Hydrazine hydrate (1:1)HCID 81531DiisopropylethylamineHCID 86667955(2,4-Dichloro-pyrimidin-5-yl)-(2-methylsulfanyl-pyrimidin-4-yl)-methanone

생성물 1

HCID 178503430HCID 178503430, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

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온도
50 °C

실험 절차

To a solution of (2,4-dichloro-pyrimidin-5-yl)-(2-methylsulfanyl-pyrimidin-4-yl)-methanone (9.52 g, 31.6 mmol) in THF (100 mL) was added hydrazine hydrate (2.3 g, 46 mmol) and DIPEA (5.9 g, 45.7 mmol). The mixture was heated at 50° C. for 4 hours, then concentrated to dryness. The resulting precipitate was collected by filtration and washed with water to give 6-chloro-3-(2-methylsulfanyl-pyrimidin-4-yl)-1H-pyrazolo[3,4-d]pyrimidine as a yellow solid. (Yield 7.8 g, 88%).

후처리

  1. concentrationconcentrated to dryness
  2. filtrationThe resulting precipitate was collected by filtration
  3. washwashed with water

출처 및 근거

ORD 기록
ord-f647dc0412a44394baa2c816168c0f4e
출처 데이터셋
uspto-grants-2013_01
특허 번호
US08362023B2

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