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Acetonitrile → 6-(7-(3-Chloropyridin-2-yl)-5,6,7,8-tetrahydropyrido[3,4-d]pyrimidin-4-ylamino)-3,3-dimethylindolin-2-one

HRID 971255
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인쇄 미리보기

반응식

HRID 971255 반응식
Cl[C:2]1[C:3]2[CH2:11][CH2:10][N:9]([C:12]3[C:17]([Cl:18])=[CH:16][CH:15]=[CH:14][N:13]=3)[CH2:8][C:4]=2[N:5]=[CH:6][N:7]=1.[NH2:19][C:20]1[CH:28]=[C:27]2[C:23]([C:24]([CH3:31])([CH3:30])[C:25](=[O:29])[NH:26]2)=[CH:22][CH:21]=1.C(#N)C.C([O-])(O)=O.[Na+]>CCOC(C)=O>[Cl:18][C:17]1[C:12]([N:9]2[CH2:10][CH2:11][C:3]3[C:2]([NH:19][C:20]4[CH:28]=[C:27]5[C:23]([C:24]([CH3:31])([CH3:30])[C:25](=[O:29])[NH:26]5)=[CH:22][CH:21]=4)=[N:7][CH:6]=[N:5][C:4]=3[CH2:8]2)=[N:13][CH:14]=[CH:15][CH:16]=1
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참가 물질

6

반응물 4

HCID 6342AcetonitrileHCID 516892Sodium BicarbonateHCID 135892296-Amino-3,3-Dimethylindolin-2-OneHCID 590214784-Chloro-7-(3-chloropyridin-2-yl)-5,6,7,8-tetrahydropyrido[3,4-d]pyrimidine

생성물 1

HCID 120041006-(7-(3-Chloropyridin-2-yl)-5,6,7,8-tetrahydropyrido[3,4-d]pyrimidin-4-ylamino)-3,3-dimethylindolin-2-one수율 66%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

반응 조건

온도
180 °C

실험 절차

A mixture of the 4-chloro-7-(3-chloropyridin-2-yl)-5,6,7,8-tetrahydropyrido[3,4-d]pyrimidine (50 mg, 0.18 mmol), 6-amino-3,3-dimethylindolin-2-one (63 mg, 0.36 mmol), and acetonitrile (3 mL) was heated in a sealed tube via at 180° C. for 60 min. The mixture was treated with EtOAc (50 mL) and sat. aq. solution of NaHCO3. The organic layer was separated and washed with brine, dried (Na2SO4), and evaporated. The residue was purified by flash chromatography over silica gel to give a light yellow solid (50 mg).

후처리

  1. customThe organic layer was separated
  2. washwashed with brine
  3. dry with materialdried (Na2SO4)
  4. customevaporated
  5. customThe residue was purified by flash chromatography over silica gel

출처 및 근거

ORD 기록
ord-58e062ab00a443a892036a2cba5f9fc3
출처 데이터셋
uspto-grants-2007_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07312330B2

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