Dichloromethane → 4-(4-Fluorobenzyl)-N-(3-methoxy-4-(4-methyl-1H-imidazol-1-yl)phenyl)-7,8-dihydro-5H-thiopyrano[4,3-d]pyrimidin-2-amine

HRID 1930600노트

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HRID 1930600 반응식
[F:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][C:9]([CH:11]2[C:16](=O)[CH2:15][CH2:14][S:13][CH2:12]2)=O)=[CH:4][CH:3]=1.[CH3:18][O:19][C:20]1[CH:21]=[C:22]([NH:32][C:33]([NH2:35])=[NH:34])[CH:23]=[CH:24][C:25]=1[N:26]1[CH:30]=[C:29]([CH3:31])[N:28]=[CH:27]1.C(=O)([O-])[O-].[K+].[K+].C(Cl)Cl>CCO.O>[F:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][C:9]2[C:11]3[CH2:12][S:13][CH2:14][CH2:15][C:16]=3[N:35]=[C:33]([NH:32][C:22]3[CH:23]=[CH:24][C:25]([N:26]4[CH:30]=[C:29]([CH3:31])[N:28]=[CH:27]4)=[C:20]([O:19][CH3:18])[CH:21]=3)[N:34]=2)=[CH:4][CH:3]=1

참가 물질

7

반응물 4

HCID 6344DichloromethaneHCID 11430Potassium CarbonateHCID 593337083-(2-(4-Fluorophenyl)acetyl)dihydro-2H-thiopyran-4(3H)-oneHCID 178493227HCID 178493227, 화합물

생성물 1

HCID 593338014-(4-Fluorobenzyl)-N-(3-methoxy-4-(4-methyl-1H-imidazol-1-yl)phenyl)-7,8-dihydro-5H-thiopyrano[4,3-d]pyrimidin-2-amine

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

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온도
60 °C

실험 절차

3-(2-(4-Fluorophenyl)acetyl)dihydro-2H-thiopyran-4(3H)-one (200 mg, 0.79 mmol), 1-(3-methoxy-4-(4-methyl-1H-imidazol-1-yl)phenyl)guanidine (194 mg, 0.79 mmol) and potassium carbonate (200 mg, 1.45 mmol) was slurrified in EtOH (5 mL) and heated to 60° C. for 16 h. DCM and water were added to the cooled reaction mixture. The organic phase was separated and dried with Mg2SO4 and then the solvent was evaporated. The crude product was used as such in next step. MS (ES+) m/z 462.2 (M+H)+

후처리

  1. customThe organic phase was separated
  2. dry with materialdried with Mg2SO4
  3. customthe solvent was evaporated

출처 및 근거

ORD 기록
ord-a14b2dcd662e4f75bef682288de3ef7e
출처 데이터셋
uspto-grants-2012_05
특허 번호
US08188101B2

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