Potassium Carbonate → HCID 69216254, 화합물

HRID 900164노트

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HRID 900164 반응식
[CH2:1]([N:4]1[C:8]2[N:9]=[CH:10][N:11]=[C:12](Cl)[C:7]=2[C:6]([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)=[C:5]1[C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1)[CH:2]=[CH2:3].[S:26]1[CH2:30][CH2:29][CH2:28][CH:27]1[CH2:31][NH2:32].C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O.CCOC(C)=O>[CH2:1]([N:4]1[C:8]2[N:9]=[CH:10][N:11]=[C:12]([NH:32][CH2:31][CH:27]3[CH2:28][CH2:29][CH2:30][S:26]3)[C:7]=2[C:6]([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)=[C:5]1[C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1)[CH:2]=[CH2:3]

참가 물질

6

반응물 3

HCID 11430Potassium CarbonateHCID 15629560Tetrahydro-2-thiophenemethanamineHCID 86603371HCID 86603371, 화합물

생성물 1

HCID 69216254HCID 69216254, 화합물

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매

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온도
120 °C

실험 절차

To a solution of 7-allyl-4-chloro-5,6-diphenyl-7H-pyrrolo[2,3-d]pyrimidine (Example 3, Step B; 200 mg, 0.58 mmol) and 140 mg of (tetrahydrothiophen-2-yl)methylamine (1.20 mmol) in N,N-dimethylformamide (3 mL) was added potassium carbonate (200 mg, 1.45 mmol). The mixture was stirred for 5 minutes at 120° C. under microwave irradiation (using powerMAX™). The reaction mixture was then cooled and diluted with EtOAc (25 mL). The mixture was extracted twice with water (10 mL) and then brine. The organic layer was dried over MgSO4, filtered and the filtrate was concentrated. The residue was purified by preparative HPLC (C8 column, water, acetonitrile, 0.1% TFA) to give the title compound.

후처리

  1. temperatureThe reaction mixture was then cooled
  2. extractionThe mixture was extracted twice with water (10 mL)
  3. dry with materialThe organic layer was dried over MgSO4
  4. filtrationfiltered
  5. concentrationthe filtrate was concentrated
  6. customThe residue was purified by preparative HPLC (C8 column, water, acetonitrile, 0.1% TFA)

출처 및 근거

ORD 기록
ord-14162b92b5d14577acf92fd1eee2df90
출처 데이터셋
uspto-grants-2008_04
특허 번호
US07358250B2

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